* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
With hydrazine hydrate In methanol at 20℃; for 1 h;
b. Quinoxalin-6-amine To a solution of 6-nitroquinoxaline (17.0 g, 0.097 mol) in MeOH (500 mL) was added hydrazine hydrate (19.4 g, 0.39 mol) and Raney Ni (2.0 g). The mixture was stirred at room temperature for 1 h. The mixture was then filtered, and the filtrate was concentrated under reduce pressure to give quinoxalin-6-amine as a yellow solid (14.0 g, yield 99percent). ESI MS: m/z 146.1 [M+H]+.
98.75%
With hydrazine hydrate In methanol at 0 - 20℃; for 2 h;
[0170] To a solution of 6-nitroquinoxaline (2.2 g, 12.57 mmol, 1.0 eq) in MeOH, was added dropwise Ranney-Ni (0.7 mL) and hydrazine hydrate (5 mL) was added at 0 °C. The mixture was stirred for 2 h at RT. The mixture was filtered and washed with MeOH. The solid was dried under vacuo to give the product (1.8 g, yield: 98.75percent>). LC/MS: m/z (M++l) = 146. 42C. Preparation of N-methylquinoxalin-6-amine
82%
With hydrogen In methanol for 4 h;
Synthesis of 3-chloro-2-methvl-N-auinoxalin-6-vl-benzenesulfonamide, STX 957:; 6-aminoquinoxaline (KRB01083) :; To a solution of 6-nitroquinoxaline [24] (500 mg, 2.86 mmol) in methanol (20 mL) was added 10percent palladium on carbon (50 mg) and the mixture was stirred under 1 atm H2 for 4 h. The mixture was filtered through celite and the filtrate evaporated. The residue was passed through a silica plug and evaporated to afford 6-aminoquinoxaline as a yellow solid (342 mg, 82percent), single spot at Rf 0.32 (ethyl acetate).'H NMR (CDCI3) : 8 8.65 (1H, d, J= 1.7 Hz), 8.55 (1H, d, J=1.7 Hz), 7.87 (1H, d, J=8. 9 Hz), 7.18 (1H, dd, J=8.9, 2.5 Hz), 7.13 (1H, d, J=2.5 Hz), 4.20 (2H, br. s,-NH2) [25].
Reference：
[1] Patent: US2012/178748, 2012, A1, . Location in patent: Page/Page column 43
[2] Patent: WO2013/6792, 2013, A1, . Location in patent: Paragraph 0170
[3] Patent: WO2005/42513, 2005, A1, . Location in patent: Page/Page column 71
[4] Heterocycles, 2007, vol. 72, p. 353 - 361
[5] Journal of Medicinal Chemistry, 2016, vol. 59, # 13, p. 6169 - 6186
[6] European Journal of Organic Chemistry, 2005, # 22, p. 4870 - 4878
[7] Tetrahedron Letters, 2010, vol. 51, # 41, p. 5402 - 5405
[8] Tetrahedron, 1990, vol. 46, # 6, p. 2089 - 2096
[9] Bioorganic and Medicinal Chemistry, 2008, vol. 16, # 6, p. 3255 - 3260
[10] Journal of the American Chemical Society, 1959, vol. 81, p. 6297,6300
[11] Bioorganic and Medicinal Chemistry Letters, 2006, vol. 16, # 4, p. 815 - 820
[12] Synthesis (Germany), 2016, vol. 48, # 19, p. 3232 - 3240
2
[ 5448-43-1 ]
[ 6298-37-9 ]
Reference：
[1] Organic Letters, 2015, vol. 17, # 23, p. 5934 - 5937
[2] Angewandte Chemie - International Edition, 2015, vol. 54, # 12, p. 3773 - 3777[3] Angew. Chem., 2015, vol. 127, # 12, p. 3844 - 3848,5
[4] Angewandte Chemie - International Edition, 2015, vol. 54, # 12, p. 3768 - 3772[5] Angew. Chem., 2015, vol. 127, # 12, p. 3839 - 3843,5
[6] Organic Letters, 2014, vol. 16, # 17, p. 4388 - 4391
3
[ 615-47-4 ]
[ 6298-37-9 ]
Reference：
[1] Patent: US6323204, 2001, B1,
[2] Patent: US5373010, 1994, A,
[3] Patent: US5077292, 1991, A,
[4] Patent: US5552403, 1996, A,
[5] Patent: US5231096, 1993, A,
[6] Patent: US5021416, 1991, A,
With hydrazine hydrate;Raney Ni; In methanol; at 20℃; for 1h;
b. Quinoxalin-6-amine To a solution of <strong>[6639-87-8]6-nitroquinoxaline</strong> (17.0 g, 0.097 mol) in MeOH (500 mL) was added hydrazine hydrate (19.4 g, 0.39 mol) and Raney Ni (2.0 g). The mixture was stirred at room temperature for 1 h. The mixture was then filtered, and the filtrate was concentrated under reduce pressure to give quinoxalin-6-amine as a yellow solid (14.0 g, yield 99%). ESI MS: m/z 146.1 [M+H]+.
98.75%
With hydrazine hydrate; In methanol; at 0 - 20℃; for 2h;
[0170] To a solution of <strong>[6639-87-8]6-nitroquinoxaline</strong> (2.2 g, 12.57 mmol, 1.0 eq) in MeOH, was added dropwise Ranney-Ni (0.7 mL) and hydrazine hydrate (5 mL) was added at 0 C. The mixture was stirred for 2 h at RT. The mixture was filtered and washed with MeOH. The solid was dried under vacuo to give the product (1.8 g, yield: 98.75%>). LC/MS: m/z (M++l) = 146. 42C. Preparation of N-methylquinoxalin-6-amine
82%
With hydrogen;palladium 10% on activated carbon; In methanol; under 760.051 Torr; for 4h;
Synthesis of 3-chloro-2-methvl-N-auinoxalin-6-vl-benzenesulfonamide, STX 957:; 6-aminoquinoxaline (KRB01083) :; To a solution of <strong>[6639-87-8]6-nitroquinoxaline</strong> [24] (500 mg, 2.86 mmol) in methanol (20 mL) was added 10% palladium on carbon (50 mg) and the mixture was stirred under 1 atm H2 for 4 h. The mixture was filtered through celite and the filtrate evaporated. The residue was passed through a silica plug and evaporated to afford 6-aminoquinoxaline as a yellow solid (342 mg, 82%), single spot at Rf 0.32 (ethyl acetate).'H NMR (CDCI3) : 8 8.65 (1H, d, J= 1.7 Hz), 8.55 (1H, d, J=1.7 Hz), 7.87 (1H, d, J=8. 9 Hz), 7.18 (1H, dd, J=8.9, 2.5 Hz), 7.13 (1H, d, J=2.5 Hz), 4.20 (2H, br. s,-NH2) [25].
The first organolithium R3Li (2.5 mmol) is added slowly to a solution of compound D (1 mmol) in anhydrous THF at -78 C. under inert atmosphere of nitrogen. The solution becomes reddish-black. The mixture is stirred at -78 C. for 2.5 h. The mixture is placed at 0 C. and the second organolithium R4Li (2 mmol) is immediately added slowly. The mixture is stirred at 0 C. for 2 h. The reaction is hydrolyzed by a saturated aqueous NH4Cl solution and extracted with ethyl acetate. The organic phase is washed with water saturated with NaCl, dried on anhydrous MgSO4 and concentrated under reduced pressure. The residue obtained is dissolved in CHCl3 (20 ml) and then MnO2 (5 mmol, 430 mg) is added and the mixture carried at reflux for 4 h. The reaction is hydrolyzed and then filtered on celite. The organic phase is dried on anhydrous MgSO4 and concentrated under vacuum. The products are purified on a silica column in a mixture of cyclohexane and ethyl acetate in a proportion of 5:5.Yield: 30%1H NMR (300 MHz, CDCl3) delta ppm: 0.96 (m, 6H); 1.31-1.32 (m, 8H); 1.40-1.52 (m, 2H); 1.68-1.79 (m, 2H); 2.9 (m, 4H); 4.10 (s, 2H); 7.05 (m, 2H); 7.74 (d, J=9.6 Hz, 1H).13C NMR (75 MHz, CDCl3) delta ppm: 13.9, 14.0, 22.5, 29.1, 29.2, 29.3, 29.4, 31.6, 35.1, 35.4, 108.0, 120.5, 129.3, 135.8, 142.5, 146.9, 152.6, 156.6.ESI-MS m/z: 286 ([M+H]+, 40).IR cm-1: 725, 830, 855, 930, 960, 1080, 1135, 1235, 1340, 1465, 1500, 1620, 2925, 2855, 2955, 3215, 3335.
palladium-carbon; In methanol; water; acetonitrile;
(a) Quinoxaline-6-ylamine. To a round-bottomed flask equipped with magnetic stirring was added 4-nitro-1,2-phenylenediamine (1.0 g, 6.5 mmol, Aldrich), acetonitrile (10 mL) and glyoxal (2.2 mL, 19 mmol, 40 wt. % in water, Aldrich). The reaction mixture was allowed to stir at 50 C. for 12 h, then concentrated in vacuo to yield 1.1 g crude <strong>[6639-87-8]6-nitro-quinoxaline</strong>. The crude product was dissolved in methanol, treated with 10% Pd/C (10 mg, Aldrich) and stirred under H2 (1 atm) at 25 C. overnight. The reaction mixture was filtered through Celite and the filtrate was concentrated in vacuo to provide the title product. MS (ESI, pos. ion) m/z: 146 (M+1).
6-Aminoquinoxaline Glyoxal sodium bisulfite adduct (Aldrich, 14.3g, 50 mmol) was added in small portions to a solution of 1,2,4-triaminobenzene dihydrochloride (9.8 g, 50 mmol) in 200 ml of 10% by weight sodium carbonate in water. The reaction mixture was heated to 100 C. for two hours and then cooled to 0 C. The crystals formed were filtered off and dried in vacuo to give a crude yield of 7.06 g (a yield of 97%) of brown crystals. Recrystallization from benzene gave 6.32 g (a yield of 87%) yellow crystals, m.p. 157-8 C. Using various analytical procedures, these yellow crystals were determined to be 6-aminoquinoxaline.
87%
In water; sodium carbonate;
6-Aminoquinoxaline Glyoxal sodium bisulfite adduct (Aldrich, 14.3g, 50 mmol) was added in small portions to a solution of 1,2,4-triaminobenzene dihydrochloride (9.8 g, 50mmol) in 200 ml of 10% by weight sodium carbonate in water. The reaction mixture was heated to 100 C. for two hours and then cooled to 0 C. The crystals formed were filtered off and dried in vacuo to give a crude yield of 7.06 g (a yield of 97%) of brown crystals. Recrystallization from benzene gave 6.32 g (a yield of 87%) yellow crystals, m.p. 157-8 C. Using various analytical procedures, these yellow crystals were determined to be 6-aminoquinoxaline.
87%
In water; sodium carbonate;
6-Aminoquinoxaline Glyoxal sodium bisulfite adduct (Aldrich, 14.3 g, 50 mmol) was added in small portions to a solution of 1,2,4-triaminobenzene dihydrochloride (9.8 g, 50 mmol) in 200 ml of 10% by weight sodium carbonate in water. The reaction mixture was heated to 100 C. for two hours and then cooled to 0 C. The crystals formed were filtered off and dried in vacuo to give a crude yield of 7.06 g (a yield of 97%) of brown crystals. Recrystallization from benzene gave 6.32 g (a yield of 87%) yellow crystals, m.p. 157-8 C. Using various analytical procedures, these yellow crystals were determined to be 6-aminoquinoxaline.
6-amino-5-bromo-quinoxaline hydrobromide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
100%
With bromine; In water-while; acetic acid;
6-Amino-5-bromoquinoxaline hydrobromide 6-Aminoquinoxaline (2.08 g, 14.4 mmol) was dissolved in 11.5 ml glacial acetic acid. The solution was cooled in water-while a solution of bromine (0.74 ml, 2.3 g, 14.4 mmol) in 1.5 ml glacial acetic acid was added slowly over 15 min. After stirring for an additional 30 min, the orange red solid formed was filtered off and washed thoroughly with dry ether. The solid was dried in vacuo overnight to yield 4.44 g crude product (a yield of 100%). The compound, 6-amino-5-bromoquinoxaline hydrobromide, had no definite melting point. A phase change (from fine powder to red crystals) was noticed at about 220 C. Decomposition was observed at about 245 C. It was used directly for the next step.
100%
With bromine; In water; acetic acid;
6-Amino-5-bromoquinoxaline hydrobromide 6-Aminoquinoxaline (2.08 g, 14.4 mmol) was dissolved in 11.5 ml glacial acetic acid. The solution was cooled in water while a solution of bromine (0.74 ml, 2.3 g, 14.4 mmol) in 1.5 ml glacial acetic acid was added slowly over 15 min. After stirring for an additional 30 min, the orange red solid formed was filtered off and washed thoroughly with dry ether. The solid was dried in vacuo overnight to yield 4.44 g crude product (a yield of 100%). The compound, 6-amino-5-bromoquinoxaline hydrobromide, had no definite melting point. A phase change (from fine powder to red crystals) was noticed at about 220 C. Decomposition was observed at about 245 C. It was used directly for the next step.
100%
With bromine; In water; acetic acid;
6-Amino-5-bromoquinoxaline hydrobromide 6-Aminoquinoxaline (2.08 g, 14.4 mmol) was dissolved in 11.5 ml glacial acetic acid. The solution was cooled in water while a solution of bromine (0.74 ml, 2.3 g, 14.4 mmol) in 1.5 ml glacial acetic acid was added slowly over 15 min. After stirring for an additional 30 min, the orange red solid formed was filtered off and washed thoroughly with dry ether. The solid was dried in vacuo overnight to yield 4.44 g crude product (a yield of 100%). The compound, 6-amino-5-bromoquinoxaline hydrobromide, had no definite melting point. A phase change (from fine powder to red crystals) was noticed at about 220 C. Decomposition was observed at about 245 C. It was used directly for the next step.
METHOD B To a stirred solution of <strong>[6298-37-9]6-aminoquinoxaline</strong> (3 g.) in glacial acetic acid at room temperature was added dropwise over a period of one minute a solution of iodine monochloride (4.5 g.) in glacial acetic acid (15 ml.). Stirring at room temperature was continued for a further 30 minutes, after which the precipitated solid was collected by filtration and washed with diethyl ether to afford 6.5 g. of 6-amino-5-iodoquinoxaline hydrochloride, as a complex with iodine, m.p. 167-169 with decomposition. Analysis: Found: C, 21.79; H, 1.58; N, 9.66%. Required for C8 H6 IN3.I.HCl: C, 22.11; H, 1.63; N, 9.67%.
6-amino-5-bromo-quinoxaline hydrobromide[ No CAS ]
[ 50358-63-9 ]
Yield
Reaction Conditions
Operation in experiment
With bromine; In water; acetic acid;
Preparation 6-amino-5-bromoquinoxaline Hydrobromide 6-Aminoquinoxaline (2.08 g, 14.4 mmol) was dissolved in 11.5 ml glacial acetic acid. The solution was cooled in water while a solution of bromine (0.74 ml, 2.3 g, 14.4 mmol) in 1.5 ml glacial acetic acid was added slowly over 15 minutes. After stirring for an additional 30 minutes, the orange red solid formed was filtered off and washed thoroughly with dry ether. The solid was dried in vacuo overnight to yield 4.44 g crude product (a yield of 100percent). The compound, 6-amino-5-bromoquinoxaline hydrobromide, had no definite melting point. A phase change from fine powder to red crystals was observed at about 2200 C. Decomposition was observed at about 2450 C. The material was used directly for preparation of 6-amino-5-bromoquinoxaline as follows.
4-propyl-N-quinoxalin-6-yl-benzenesulfonamide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
94%
Synthesis of 4-propvl-N-quinoxalin-6-vl-benzenesulfonamide, STX 958 (KRB01085) :; To a solution of 4n-propylbenzenesulphonyl chloride (142 mg, 0.651 mmol) in dichloromethane (4 mL) was added pyridine (125 uL, 1.55 mmol) and the mixture was stirred under N2 for 5 min, after which time <strong>[6298-37-9]6-aminoquinoxaline</strong> (90 mg, 0.62 mmol) was added. The resulting mixture was stirred for 4 h at room temperature, then saturated NaHCO3 solution (10 mL) was added and the mixture was extracted into ethyl acetate (20 mL). The organic phase was washed with brine, dried (Na2SO4), filtered and evaporated to give a residue that was purified using flash chromatography to afford an off-white solid (190 mg, 94%), single spot at Rf 0.66 (ethyl acetate). mp 198. 4-198. 9C, HPLC purity 99+% (tR 2. 22 min in 10% water-acetonitrile).'H NMR (CDCI3) : 68. 77 (1H, d, J=1.7 Hz), 8.73 (1H, d, J=1.7 Hz), 8.00 (1H, d, J=8.9 Hz), 7.80 (2H, d, J=8.2 Hz), 7.71 (1 H, d, J=2.5 Hz), 7.59 (1H, dd, J=8.9, 2.5 Hz), 7.23 (2H, obscured under CHCl3), 2.57 (2H, t, J=7.6 Hz), 1.58 (2H, sextet, J=7.5 Hz), 0.87 (3H, t, J=7.4 Hz). LCMS: 326.24 (M- ). FAB-MS (MH+, C17H17N302S) : calcd 328.1119, found 328.1136.
3-chloro-2-methyl-N-quinoxalin-6-yl-benzenesulfonamide[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
87%
To a solution of 3-chloro-2-methylbenzenesulphonyl chloride (147 mg, 0.651 mmol) in dichloromethane (4 mL) was added pyridine (125 muL, 1.55 mmol) and the mixture was stirred under N2 for 5 min, after which time <strong>[6298-37-9]6-aminoquinoxaline</strong> (90 mg, 0.62 mmol) was added. The resulting mixture was stirred for 5 h at room temperature, then saturated NaHCO3 solution (10 mL) was added and the mixture was extracted into ethyl acetate (20 mL). The organic phase was washed with brine, dried (Na2SO4), filtered and evaporated to give a residue that was purified using flash chromatography to afford a pale yellow solid (180 mg, 87%), single spot at Rf 0.60 (ethyl acetate). mp 166.5- 166. 9C, HPLC purity 99+% (tR 2.15 min in 10% water-acetonitrile). 1H NMR (CDCI3) : 5 8.77 (1 H, d, J=1. 7 Hz), 8.74 (1H, d, J=1. 7 Hz), 8.06 (1H, d, J=8.2 Hz), 8.00 (1H, d, J=9. 2 Hz), 7.66 (1H, d, J=2.5 Hz), 7.56 (1H, d, J=7.9 Hz), 7.50 (1H, dd, J=9.1, 2.6 Hz), 7.28- 7.22 (1H, obscured under CHC13), 2.76 (3H, s). LCMS: 332.24 (M-). FAB-MS (MH+, C15H12CIN302S) : calcd 334.0417, found 334.0433.
To a solution of compound D or E (1 mmol) in dichloromethane (10 ml) at 0 C. under atmosphere of nitrogen are added triethylamine (0.55 ml, 2 mmol) and slowly the acid chloride in solution in dichloromethane (5 ml). The reaction mixture is stirred at room temperature for 2 h. The reaction is hydrolyzed with water and then extracted with dichloromethane. The organic phase is dried on anhydrous MgSO4 and then concentrated under vacuum. The products are purified on a silica column in a mixture of cyclohexane and ethyl acetate in a proportion of 8:2.Yield: 70%1H NMR (300 MHz, CDCl3) delta ppm: 0.88 (t, J=6.9 Hz, 3H); 1.25 (m, 18H); 1.68 (m, 6H); 2.45 (t, J=7.5 Hz, 2H); 7.58 (s, 1H); 8.04 (m, 2H); 8.27 (s, 1H); 8.74 (d, J=1.5 Hz, 1H); 8.79 (d, J=1.5 Hz, 1H).13C NMR (50 MHz, CDCl3) delta ppm: 14.1, 22.7, 25.5, 29.4, 29.5, 29.6, 31.9, 37.9, 116.8, 124.0, 130.1, 139.5, 140.2, 143.7, 145.4, 171.9.ESI-MS m/z: 370 ([M+H]+, 100).IR cm-1: 732, 786, 832, 957, 1026, 1217, 1355, 1498, 1542, 1583, 1619, 1671, 1749, 2851, 2921, 3054, 3304
To a solution of <strong>[6298-37-9]6-aminoquinoxaline</strong> (290 mg, 2 mmol) and hydroxypentadecanoic acid (518 mg, 2 mmol) in dichloromethane (40 ml) are added triethylamine (0.83 ml, 6 mmol), EDC (768 mg, 4 mmol) and HOBt (405 mg, 3 mmol). The mixture is stirred overnight at room temperature under inert atmosphere of nitrogen. The reaction is hydrolyzed, extracted with dichloromethane and then washed with a concentrated NH4Cl solution. The organic phase is dried on anhydrous MgSO4 and concentrated under reduced pressure. The residue obtained is then dissolved in DMF (10 ml), and then imidazole (136 mg, 2 mmol) and TBDMS-Cl (332 mg, 2.2 mmol) are added. The mixture is stirred overnight at room temperature under inert atmosphere of nitrogen. The reaction is hydrolyzed and then extracted with ethyl acetate, dried on anhydrous MgSO4 and concentrated under vacuum. The silylated product is purified on a silica column in a mixture of cyclohexane and ethyl acetate in a proportion of 8:2. The product is then dissolved in THF (10 ml) and TBAF (3 ml, 1 M in THF) is added. After 5 minutes the reaction is hydrolyzed and extracted with ethyl acetate. The organic phase is dried on anhydrous MgSO4 and concentrated under vacuum. The product is obtained with a total yield of 38% on three steps.
[0171] To a solution of NaOCH3 (3.35 g, 62.07 mmol, 5.0 eq) in MeOH (60 mL), was added <strong>[6298-37-9]quinoxalin-6-amine</strong> (1.8 g, 12.41 mmol, 1.0 eq) and (HCHO)n (558.6 mg, 18.62 mmol, 1.5 eq). The mixture was heated to 50 C overnight. After cooling, NaBH4 (943.5 mg, 24.83 mmol, 2.0 eq) was added portwise, and the mixture was stirred at RT for 2 h. The resulting mixture was concentrated and the residue was dissolved in EtOAc, washed with water (3 times), dried over Na2S04 and concentrated under vacuo. The crude product was purified by chromatograph on silica gel (PE:EA = from 5: 1, to 0: 1, gradient ) to give the product (700 mg, yield: 35.5%); LC/MS: m/z (M++l) = 160.
With N-ethyl-N,N-diisopropylamine; In acetonitrile; at 200℃; for 0.5h;Microwave irradiation;
General procedure: A mixture of an a-halogenoketone, an amine and a base (DIPEA or triethylamine) in a solvent (e.g. DMF, ethanol, acetonitrile, dioxane or THF) was irradiated in a microwave oven at 100C to 200C (more in particular at 120 to 200 C) for 5 to 180 min. (more in particular for 15 to 120 min). The reaction mixture was concentrated under reduced pressure and the residue was purified by flash chromatography on silica gel.
With triethylamine; In dichloromethane; acetonitrile; at 0 - 20℃;
General procedure: Procedure A: The isothiocyanate compound (1 equiv) was added to the solution of amine (1 equiv) in 5 ml of a mixture of dichloromethane and acetonitrile (1:1, v/v). The mixture was cooled to 0C. Then, triethylamine (2 equiv) was added gradually. The mixture was stirred at 0C for 15 min, after which stirring was continued at room temperature for 2-10 h. The reaction mixture was concentrated, extracted with dichloromethane, and washed with brine.The organic layer was dried over MgSO4 and purified by column chromatography (MeOH/CH2Cl2) or by preparative TLC (MeOH/CH2Cl2) to afford the desired product.
4-((quinoxalin-6-ylamino)methyl)-1H-pyrazole-5-carboxylic acid[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
Synthesis of 4-((quinoxalin-6-ylamino)methyl)-1H-pyrazole-5-carboxylic acid (5-B) To a suspension of product (4-B) (100 mg, 0.71 mmol) and <strong>[6298-37-9]quinoxalin-6-amine</strong> (104 mg, 0.71 mmol) in a solution of 1,2-dichloroethane (DCE, 5 mL) and DMF (5 mL) was added acetic acid (5 drops) at rt. The reaction mixture was then stuffed for 16 h. MeOH (5 mL) was added, followed by NaBH4 (100 mg, 2.63 mmol). The reaction mixture was stuffed at rt for another 30 mm.The solution was diluted with ethyl acetate (30 mL); washed with 5 % citric acid (10 mL) and brine (20 mL); dried over Na2504 and concentrated to give crude product (5-B) (200 mg, 99 %) as a yellow solid. LC-MS (M+H) = 270.
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