Reference：
[1] Angewandte Chemie, International Edition, 2009, vol. 48, # 33, p. 6097 - 6100[2] Angewandte Chemie, 2009, vol. 121, # 33, p. 6213 - 6216
2
[ 1679-64-7 ]
[ 7377-26-6 ]
Yield
Reaction Conditions
Operation in experiment
95%
for 15 h; Heating / reflux
4-Chlorocarbonyl-benzoic acid methyl ester (2).; To a mixture of Terephtalic acid monomethyl ester, compound 1 (lo.oog, 0.056 mol) and SOCl2 (somL) was added a drop of DMF and the mixture was boiled at refluxed for 15I1. The excess SOCl2 was removed in vacuo to afford compound 2 (io.57g) as a white solid in 95percent yield. This compound was used for the next step without further purification.
93%
for 1 h; Reflux
Reaction conditions to obtain compound 49 (4-Chlorocarbonyl-benzoic acid methyl ester): Terephthalic acid monomethyl ester (0.25 g, 1.4 mmol) was dissolved in thionyl chloride (5 ml) and refluxed for 1 hour. Excess thionyl chloride was removed in vacuo to give an off-white solid. The solid was dissolved in anhydrous benzene (7 ml), and the solvent was evaporated. The procedure was repeated 3 times, and the solid was dried at high temperatures to remove residual solvent. 273 mg was obtained at 93percent yield.
Reference：
[1] Journal of the American Chemical Society, 1995, vol. 117, # 27, p. 7041 - 7047
[2] Patent: WO2009/37302, 2009, A1, . Location in patent: Page/Page column 24
[3] Organic Letters, 2017, vol. 19, # 15, p. 4142 - 4145
[4] Patent: US2015/158888, 2015, A1, . Location in patent: Paragraph 0114
[5] Journal of Organic Chemistry, 2005, vol. 70, # 7, p. 2763 - 2770
[6] Journal of Medicinal Chemistry, 2011, vol. 54, # 23, p. 8099 - 8109
[7] Journal of Organic Chemistry, 1974, vol. 39, # 23, p. 3384 - 3387
[8] Makromolekulare Chemie, 1957, vol. 23, p. 31,51[9] Angewandte Chemie, 1955, vol. 67, p. 108
[10] Journal of Medicinal Chemistry, 1983, vol. 26, # 8, p. 1164 - 1168
[11] Bulletin of the Chemical Society of Japan, 1992, vol. 65, # 10, p. 2807 - 2813
[12] Magnetic Resonance in Chemistry, 1989, vol. 27, # 6, p. 585 - 591
[13] Journal of Physical Chemistry, 1988, vol. 92, # 16, p. 4801 - 4806
[14] Gazzetta Chimica Italiana, 1987, vol. 117, # 9, p. 529 - 532
[15] Canadian Journal of Chemistry, 1994, vol. 72, # 1, p. 142 - 145
[16] Journal of Medicinal Chemistry, 1995, vol. 38, # 1, p. 58 - 67
[17] Journal of Medicinal Chemistry, 1994, vol. 37, # 26, p. 4538 - 4553
[18] Journal of Organic Chemistry, 1996, vol. 61, # 4, p. 1297 - 1301
[19] Journal of Organic Chemistry USSR (English Translation), 1986, vol. 22, p. 620 - 627[20] Zhurnal Organicheskoi Khimii, 1986, vol. 22, # 4, p. 694 - 701
[21] J. Gen. Chem. USSR (Engl. Transl.), 1983, vol. 53, # 11, p. 2258 - 2262[22] Zhurnal Obshchei Khimii, 1983, vol. 53, # 11, p. 2505 - 2510
[23] Bioorganic and Medicinal Chemistry Letters, 1999, vol. 9, # 2, p. 227 - 232
[24] Archiv der Pharmazie, 2002, vol. 335, # 2-3, p. 83 - 88
[25] Journal of Medicinal Chemistry, 2004, vol. 47, # 18, p. 4360 - 4372
[26] Archiv der Pharmazie, 2006, vol. 339, # 3, p. 115 - 122
[27] Journal of Medicinal Chemistry, 2006, vol. 49, # 2, p. 748 - 759
[28] Synthesis, 2006, # 3, p. 509 - 513
[29] Journal of the American Chemical Society, 2001, vol. 123, # 20, p. 4849 - 4850
[30] Chemistry - A European Journal, 2002, vol. 8, # 5, p. 1015 - 1023
[31] Angewandte Chemie - International Edition, 2007, vol. 46, # 4, p. 576 - 579
[32] Bioorganic and Medicinal Chemistry, 2006, vol. 14, # 24, p. 8590 - 8598
[33] Patent: US2005/85512, 2005, A1, . Location in patent: Page/Page column 13
[34] Patent: EP1541549, 2005, A1, . Location in patent: Page/Page column 15
[35] Patent: US5324859, 1994, A,
[36] Patent: US5534531, 1996, A,
[37] Patent: WO2007/67836, 2007, A2, . Location in patent: Page/Page column 142
[38] Chemistry - A European Journal, 2008, vol. 14, # 4, p. 1238 - 1252
[39] Chemistry - A European Journal, 2008, vol. 14, # 10, p. 3146 - 3153
[40] Patent: US2009/131468, 2009, A1, . Location in patent: Page/Page column 25-26
[41] Patent: WO2009/64251, 2009, A1, . Location in patent: Page/Page column 36-37
[42] Patent: WO2009/64251, 2009, A1, . Location in patent: Page/Page column 38-39
[43] Chemistry - A European Journal, 2009, vol. 15, # 7, p. 1637 - 1648
[44] Journal of the American Chemical Society, [45] Journal of the American Chemical Society, 2009, vol. 131, p. 6898 - 6899
[46] Patent: WO2004/89916, 2004, A1, . Location in patent: Page 26
[47] Journal of Medicinal Chemistry, 2009, vol. 52, # 19, p. 5950 - 5966
[48] Patent: EP2189450, 2010, A1, . Location in patent: Page/Page column 14
[49] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, # 24, p. 6882 - 6889
[50] Patent: EP2202229, 2010, A1, . Location in patent: Page/Page column 26
[51] Angewandte Chemie - International Edition, 2011, vol. 50, # 28, p. 6379 - 6382
[52] Patent: WO2011/73231, 2011, A1, . Location in patent: Page/Page column 98
[53] Journal of Materials Chemistry, 2011, vol. 21, # 16, p. 5916 - 5922
[54] Patent: WO2011/141928, 2011, A1, . Location in patent: Page/Page column 18-19
[55] Organic Letters, 2012, vol. 14, # 2, p. 656 - 659
[56] Organic Letters, 2012, vol. 14, # 1, p. 354 - 357
[57] Molecular Crystals and Liquid Crystals, 2011, vol. 551, p. 60 - 68
[58] Journal of the American Chemical Society, 2012, vol. 134, # 20, p. 8298 - 8301
[59] Organic Letters, 2012, vol. 14, # 12, p. 3044 - 3047
[60] Angewandte Chemie - International Edition, 2012, vol. 51, # 29, p. 7318 - 7322
[61] Journal of the American Chemical Society, 2012, vol. 134, # 29, p. 11948 - 11951
[62] Organic and Biomolecular Chemistry, 2013, vol. 11, # 6, p. 881 - 885
[63] Patent: WO2012/171903, 2012, A1, . Location in patent: Page/Page column 50
[64] Chemistry - A European Journal, 2013, vol. 19, # 4, p. 1373 - 1384
[65] Beilstein Journal of Organic Chemistry, 2013, vol. 9, p. 97 - 105
[66] Bioorganic and Medicinal Chemistry Letters, 2013, vol. 23, # 8, p. 2313 - 2318
[67] Journal of the American Chemical Society, 2013, vol. 135, # 12, p. 4628 - 4631
[68] Synthesis (Germany), 2013, vol. 45, # 16, p. 2234 - 2240
[69] Medicinal Chemistry Research, 2013, vol. 22, # 8, p. 3857 - 3862
[70] European Journal of Organic Chemistry, 2013, # 27, p. 6137 - 6145
[71] Organic Letters, 2014, vol. 16, # 2, p. 390 - 393
[72] Journal of Materials Chemistry C, 2014, vol. 2, # 34, p. 7029 - 7038
[73] Bioorganic and Medicinal Chemistry, 2014, vol. 22, # 19, p. 5487 - 5505
[74] Tetrahedron Letters, 2014, vol. 55, # 44, p. 6044 - 6047
[75] Chemical Communications, 2015, vol. 51, # 1, p. 77 - 80
[76] Organic Letters, 2014, vol. 16, # 24, p. 6412 - 6415
[77] Journal of Medicinal Chemistry, 2015, vol. 58, # 3, p. 1380 - 1389
[78] Chemical Communications, 2015, vol. 51, # 24, p. 5089 - 5092
[79] European Journal of Medicinal Chemistry, 2015, vol. 95, p. 127 - 135
[80] Chemical Communications, 2014, vol. 50, # 84, p. 12718 - 12721
[81] Journal of Organometallic Chemistry, 2015, vol. 794, p. 136 - 145
[82] Chemistry - A European Journal, 2015, vol. 21, # 30, p. 10851 - 10869
[83] Bioorganic and Medicinal Chemistry, 2015, vol. 23, # 19, p. 6510 - 6519
[84] Patent: US2015/238558, 2015, A1, . Location in patent: Paragraph 0413
[85] Patent: US2015/329556, 2015, A1, . Location in patent: Paragraph 2069-2072
[86] Organic and Biomolecular Chemistry, 2016, vol. 14, # 5, p. 1599 - 1610
[87] Advanced Synthesis and Catalysis, 2016, vol. 358, # 5, p. 746 - 751
[88] Patent: WO2016/34673, 2016, A1, . Location in patent: Page/Page column 69-70
[89] Journal of Organic Chemistry, 2016, vol. 81, # 5, p. 2166 - 2173
[90] Letters in Drug Design and Discovery, 2016, vol. 13, # 8, p. 729 - 733
[91] Molecules, 2017, vol. 22, # 1,
[92] Journal of the American Chemical Society, 2017, vol. 139, # 5, p. 1762 - 1765
[93] Patent: US2016/333004, 2016, A1, . Location in patent: Paragraph 0314; 0319
[94] Angewandte Chemie - International Edition, 2017, vol. 56, # 9, p. 2482 - 2486[95] Angew. Chem., 2017, vol. 129, # 9, p. 2522 - 2526,5
[96] Organic Letters, 2017, vol. 19, # 6, p. 1294 - 1297
[97] Journal of Organic Chemistry, 2017, vol. 82, # 1, p. 420 - 430
[98] European Journal of Organic Chemistry, 2017, vol. 2017, # 20, p. 2866 - 2870
[99] Journal of Organic Chemistry, 2017, vol. 82, # 10, p. 5046 - 5067
[100] Organic Letters, 2017, vol. 19, # 12, p. 3091 - 3094
[101] Journal of Medicinal Chemistry, 2017, vol. 60, # 14, p. 6205 - 6219
[102] Bioorganic and Medicinal Chemistry Letters, 2017, vol. 27, # 20, p. 4770 - 4776
[103] Organic Letters, 2017, vol. 19, # 19, p. 5304 - 5307
[104] Chemical Communications, 2017, vol. 53, # 93, p. 12584 - 12587
[105] Organic Process Research and Development, 2017, vol. 21, # 5, p. 748 - 753
[106] Synlett, 2017, vol. 28, # 19, p. 2594 - 2598
3
[ 1679-64-7 ]
[ 1147550-11-5 ]
[ 7377-26-6 ]
Reference：
[1] Journal of Medicinal Chemistry, 2012, vol. 55, # 7, p. 3331 - 3341
4
[ 1679-64-7 ]
[ 32529-79-6 ]
Reference：
[1] Bioorganic and Medicinal Chemistry Letters, 2009, vol. 19, # 6, p. 1564 - 1568
Reference：
[1] Patent: US7115750, 2006, B1, . Location in patent: Page/Page column 77
[2] Journal of Medicinal Chemistry, 2013, vol. 56, # 4, p. 1772 - 1776
[3] Chemistry - A European Journal, 2013, vol. 19, # 45, p. 15101 - 15104
7
[ 1679-64-7 ]
[ 39895-56-2 ]
Reference：
[1] Journal of the American Chemical Society, 1957, vol. 79, p. 672,674
8
[ 1679-64-7 ]
[ 94497-51-5 ]
Reference：
[1] Letters in Drug Design and Discovery, 2016, vol. 13, # 8, p. 729 - 733
[2] Organic Process Research and Development, 2017, vol. 21, # 5, p. 748 - 753
9
[ 1679-64-7 ]
[ 56893-25-5 ]
Reference：
[1] Journal of Medicinal Chemistry, 1983, vol. 26, # 8, p. 1164 - 1168
EXAMPLE 2 Synthesis of mono-tert-butyl terephthalate In the same manner as in Example 1, 10 g (0.056 mol) of monomethyl terephthalate and 200 ml (2.081 mols) of tert-butyl alcohol were charged, and 8.10 g (0.070 mol, 1.3 equivalent) of potassium-tert-butoxide was poured thereinto little by little at room temperature. As a result, the reaction mixture generated heat to result in rising of the temperature to 35 C., and white crystals were precipitated in the reaction mixture. Thereafter, the reaction mixture was heated to 83 C. and the reaction was carried out for 17 hours, during which methyl alcohol produced by the transesterification was distilled off together with tert-butyl alcohol, and tert-butyl alcohol in the same amount as the amount of the distilled tert-butyl alcohol was continuously added through the dropping funnel. After completion of the transesterification, tert-butyl alcohol was distilled off under normal pressure, and the residue was allowed to stand for cooling. Then, 80 ml of ice water was added to the residue, followed by separation washing twice with 100 ml of n-hexane. To the resulting aqueous phase was added 3.85 g (0.036 mol, 1.4 equivalent) of sulfuric acid diluted with 20 ml of cold water to liberate the acid. The components in the aqueous phase were analyzed by GC to obtain a peak area ratio of 66:34 of the starting monomethyl terephthalate and the product mono-tert-butyl terephthalate. This aqueous phase was subjected to extraction twice with 100 ml of n-hexane, and then the n-hexane phase extracted twice was washed thrice with 10 ml of pure water and thereafter subjected to concentration under reduced pressure. As a result, 2.99 g of mono-tert-butyl terephthalate of 94% in purity containing no monomethyl terephthalate was obtained. The yield in this case was 23%. Spectrum data of 1H-NMR on the product were as follows. 1H-NMR(CDCl3) 1.62 (9H, s), 8.08 (2H, d, J=8.1 Hz), 8.16 (2H, d, J=8.1 Hz).
7
[ 79-37-8 ]
[ 1679-64-7 ]
[ 23754-46-3 ]
[ 23754-45-2 ]
Yield
Reaction Conditions
Operation in experiment
2 g (37%)
With pyridine; In methanol; dichloromethane; benzene;
EXAMPLE 27 STR31 4-(Methylaminocarbonyl)benzoic acid. Monomethylterephthalate (Aldrich, 5.0 g, 0.028 mol) was added to 80 mL of dry benzene in a 250-mL round-bottom flask under argon and fitted with a calcium chloride drying tube. Dry pyridine (4.4 g, 0.056 mol) was added and the mixture was stirred for 15 min. Oxalyl chloride (3.66 g, 0.029 mol) was added by drop over 10 min. The mixture bubbled vigorously during the addition and a heavy white precipitate formed. The mixture was vigorously stirred for 40 min and followed by TLC (three solvent systems: dichloromethane, 2% methanol, and 5% methanol). Anhydrous methylamine was bubbled into the mixture for 10 min. The precipitate dissipated somewhat and the solution color changed from colorless to green and finally to yellow. The mixture was then stirred overnight. The remaining white precipitate was collected on a filter and washed with benzene. The filtrate was washed with water and dried over sodium sulfate. The drying agent was removed by filtration, washed with benzene, and the solvent concentrated to give a white solid. The solids were combined and dissolved in 300 mL dichloromethane. The solution was washed 3 times with 5% HCl, 3*5% sodium bicarbonate, 3*water, 1*brine, and then dried over sodium sulfate. The drying agent was removed by filtration and the filtrate concentrated to give a white solid which was dried in vacuo. This white solid was recrystallized from methanol to give 2 g (37%) of methyl 4-(methylaminocarbonyl)benzoate, mp 126 C. Analysis: Calculated for C10 H11 NO3 (193.202): C, 62.17; H, 5.74; N, 7.25 Found: C, 62.16; H, 5.74: N, 7.25
methyl 4-(1-(benzyloxy)-3-hydroxy-1-oxopropan-2-ylcarbamoyl)benzoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
74%
With 1-ethyl-(3-(3-dimethylamino)propyl)-carbodiimide hydrochloride; triethylamine; In dichloromethane;Inert atmosphere;
General procedure: L-Serine methyl ester hydrochloride 6a,b (1.0 equiv) was dissolved in CH2Cl2 together with acids 7a,b (1.1 equiv), Et3N (1.1 equiv) and EDC (1.1 equiv). After stirring overnight, the solution was washed with H2O, NaHCO3 satd sol and brine, then dried over Na2SO4. Evaporation of the solvent gave amide 8a-d, which were used without further purification.
Synthesis 12i-Dichloro-4-ethoxyphenylcarbamoyl)benzoic acid (AAA-013)ii) LiOH, THF/H20Step (i): 4-(3,5-Dichloro-4-hydroxyphenylcarbamoyl)benzoic acid (4)ii) LiOH, THF/H20A mixture of 4-(chlorocarbonyl)benzoic acid methyl ester (1) (600 mg, ca. 3.02 mmol) contaminated with 4-(methoxycarbonyl)benzoic acid was suspended in DCM (5 mL) and cooled to 0°C. The mixture was treated with oxalyl chloride (529 pL, 6.04 mmol) and DMF (1 drop). The resultant mixture was warmed to RT, stirred for 2 h, and then concentrated in vacuo. The residue was dissolved in DCM (3 mL) and a suspension of 4- amino-2,6-dichlorophenol (2) (51 1 mg, 2.9 mmol) in DCM (18 mL) was added. The resultant suspension was treated with DIPEA (1.58 mL, 9.06 mmol) and was stirred at RT overnight. The solvent was removed in vacuo and the residue partitioned between EtOAc/DCM and aqueous HCl (1 M). The layers were separated and the organic layer was washed with water and brine. The organic layer was dried over MgS04l filtered and then the solvent evaporated in vacuo to afford a pale brown solid (930 mg), which was triturated in hot acetonitrile/methanol (9: 1 ) and filtered. The precipitate and filtrate were recombined, the solvent was evaporated in vacuo and then the residue was dissolved in THF (40 mL). Water (10 mL) was added and the mixture treated with lithium hydroxide (340 mg, 14.2 mmol). The mixture was stirred overnight and then partitioned between EtOAc and aqueous HCl (1 M). The organic layer was washed successively with water (2 x 50 mL), brine, dried over MgS04, filtered and then concentrated in vacuo to afford crude 4-(3,5-dichloro-4-hydroxyphenylcarbamoyl)benzoic acid (3) as a pale brown solid. This material was used in the subsequent reaction step without purification.
A mixture of 4-(chlorocarbonyl)benzoic acid methyl ester (1) (600 mg, ca. 3.02 mmol) contaminated with 4-(methoxycarbonyl)benzoic acid was suspended in DCM (5 mL) and cooled to 0° C. The mixture was treated with oxalyl chloride (529 muL, 6.04 mmol) and DMF (1 drop). The resultant mixture was warmed to RT, stirred for 2 h, and then concentrated in vacuo. The residue was dissolved in DCM (3 mL) and a suspension of <strong>[5930-28-9]4-amino-2,6-dichlorophenol</strong> (2) (511 mg, 2.9 mmol) in DCM (18 mL) was added. The resultant suspension was treated with DIPEA (1.58 mL, 9.06 mmol) and was stirred at RT overnight. The solvent was removed in vacuo and the residue partitioned between EtOAc/DCM and aqueous HCl (1 M). The layers were separated and the organic layer was washed with water and brine. The organic layer was dried over MgSO4, filtered and then the solvent evaporated in vacuo to afford a pale brown solid (930 mg), which was triturated in hot acetonitrile/methanol (9:1) and filtered. The precipitate and filtrate were recombined, the solvent was evaporated in vacuo and then the residue was dissolved in THF (40 mL). Water (10 mL) was added and the mixture treated with lithium hydroxide (340 mg, 14.2 mmol). The mixture was stirred overnight and then partitioned between EtOAc and aqueous HCl (1 M). The organic layer was washed successively with water (2.x.50 mL), brine, dried over MgSO4, filtered and then concentrated in vacuo to afford crude 4-(3,5-dichloro-4-hydroxyphenylcarbamoyl)benzoic acid (3) as a pale brown solid. This material was used in the subsequent reaction step without purification.
Example 1: Preparation of methyl [4-(5,6,7,8-tetrahydro-3,5,5,8,8-pentamethyl-2- naphthalenyl)carbonyl]benzoateTo a solution of 4-carboxy benzoic acid (100 g) in dichloromethane (800 ml) under nitrogen gas atmosphere, phosphorous pentachloride (200 g) was added at 25-30 C and temperature was slowly raised to 38-44 C. After completion of the reaction (monitored by GC), the reaction mass was cooled to -5 to -10 C. Thereafter aluminium chloride (340g) and l,2,3,4,-tetrahydro-l-l,4,4,6-pentamethyl naphthalene (120 g) were successively added to the reaction mixture and heated slowly to 38-44C and refluxed for 1 hour. After completion of reaction (monitored by TLC), the reaction mass was cooled to 15-20 C and poured into 5N hydrochloric acid (1L). Layers were separated and aqueous layer was extracted with dichloromethane (600 ml). The combined organic layer was washed successively with demineralized water (2 L) and sodium bicarbonate solution (8 % solution, 1600 ml)) The resulting organic layer was distilled off at atmospheric pressure to give residue which was dried to give title compound having purity 98.58 %, impurity A: 0.52 % and keto acid impurity B: 0.22 % by HPLC. Purification:n-Heptane (400 ml) was added to the resulting product and stirred for 30 minutes. The mixture is then cooled to 5-10 C, stirred for 1 hour and filtered. The solid, thus obtained, is slurry washed with cold n- heptane (200 ml) and dried at 65C to give 173 g of title compound as white to off white crystalline powder having purity 99.75%, impurity A: 0.14 % and keto acid impurity B: 0.02% by HPLC.
Intermediate 74 Methyl 4-(3-ethoxy-3-oxopropanoyl)benzoate A solution of 4-(methoxycarbonyl)benzoic acid (3 g, 16.65 mmol) and 1,1'-carbonyldiimidazole (3.2 g, 19.73 mmol) in THF (50 ml) was stirred for 3 hours at 50 C. Then, a solution of the magnesium salt of malonic acid monoethyl ester (prepared via the addition of Et3N (4.3 g, 42.49 mmol) and MgCl2 (5.2 g, 58.51 mmol) to a solution of potassium 3-ethoxy-3-oxopropanoate (7.8 g, 45.88 mmol) in acetonitrile (100 ml) stirred at room temperature for 2.5 h) was added at 0 C. The resulting solution was stirred overnight at 85 C., quenched by the addition of water (100 ml) and adjusted to pH 7 with HCl (3N). The resulting solution was extracted with ethyl acetate (3*100 ml), and the organic layers were combined, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give a residue, which was purified by silica gel column chromatography with 2%-10% ethyl acetate in petroleum ether to afford methyl 4-(3-ethoxy-3-oxopropanoyl)benzoate as a white solid (2.6 g, 62%). LC/MS (ES, m/z): [M+H]+ 251.0 1H-NMR (300 MHz, CDCl3): delta 12.56 (s, 1H), 7.99-8.16 (m, 6H), 7.83-7.90 (m, 2H), 5.74 (s, 1H), 4.25-4.32 (m, 4H), 4.02-4.23 (m, 2H), 3.97 (s, 6H), 1.26-1.37 (m, 6H).
methyl 4-[(3,5-dimethyl-1,2-oxazol-4-yl)carbamoyl]benzoate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
75%
Example 45A Methyl 4-[(3,5-dimethyl-1,2-oxazol-4-yl)carbamoyl]benzoate 300 mg (1.67 mmol) of monomethyl terephthalate were dissolved in 3 ml of DMF, and 377 mg (1.97 mol) of EDC and 266 mg (1.97 mmol) of HOBT were added. The mixture was left to stir at RT for 20 min and then 170 mg (1.51 mmol) of 4-amino-3,5-dimethylisoxazole were added. The mixture was stirred at RT overnight. After dilution with water, the mixture was extracted three times with in each case 10 ml of ethyl acetate. The combined organic phases were dried over sodium sulphate, filtered and concentrated under reduced pressure. The crude product was purified chromatographically [Method 16]. This gave 342 mg (75% of theory) of the target compound. LC-MS [Method 8]: Rt=0.88 min; MS (ESI+): m/z=275 (M+H)+.
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