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CAS No. : | 13215-72-0 | MDL No. : | MFCD30543297 |
Formula : | C20H14O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | KFHMRRYUOBRPAA-UHFFFAOYSA-N |
M.W : | 318.32 | Pubchem ID : | 12378414 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P233-P260-P261-P264-P270-P271-P280-P301+P312-P302+P352-P304-P304+P340-P305+P351+P338-P312-P321-P330-P332+P313-P337+P313-P340-P362-P403-P403+P233-P405-P501 | UN#: | |
Hazard Statements: | H302-H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With sodium hypobromide In 1,4-dioxane |
Yield | Reaction Conditions | Operation in experiment |
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(i) aq. NaOH, HMPT, (ii) /BRN= 969135/; Multistep reaction; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
Multi-step reaction with 2 steps 1: AlCl3 / CH2Cl2 / -10 - 18 °C 2: aq. NaOBr / dioxane |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
54% | In water; N,N-dimethyl-formamide UO2(NO3)2*6H2O dissolved in H2O, layered with DMF/H2O 1:1 buffer layer, layered with 1.3 equiv. of ligand in DMF; crystd. at room temp. for 1 month, elem. anal.; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In methanol; N,N-dimethyl acetamide at 130℃; for 72h; | DCPB (0.03 g, 0.08 mmol), DMA (5 ml), CH3OH (5 ml) and concentratedHCl (0.2 ml) were placed in a 20 ml Teflon-lined autoclavewhich was kept at 130 C for 3 days and then slowly cooled toroom temperature at about 4 C/h. Several purple block crystals of CIAC-205 were obtained. Elemental analysis (%): C 57.38, H 4.74;found: C 59.28, H 4.23. The EDS analysis reveals that the molar ratioof Co, S and Cl molar is 5.61: 5.48: 1.47, comparable to the expectedvalue 4: 4: 1. FT-IR (cm1): 3288(w), 3051(w), 2963(s),2855(w), 1934(w), 1589(s), 1548(s), 1439(s), 1399(s), 1304(w),1250(s), 1168(s), 1087(s), 1006(s), 844(s), 763(s), 701(s), 648(m),485(s), 451(s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
78% | In dimethyl sulfoxide at 100℃; for 72h; Sealed tube; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
40% | In water; N,N-dimethyl-formamide at 85℃; for 72h; | Syntheses of compounds 1-2 Fig. S1 ). Synthesis of [Zn(TPPBDA)1/2(tpdc)]·DMF}n (2): Compound 2 was synthesized by dissolving 0.05 mmol of TPPBDA and 0.1 mmol of H2tpdc in DMF (3 mL) in a 10 mL glass vial. A solution of 2 mL 0.1 mmol aqueous Zn(NO3)2 solution was then added and the solution heated at 85 °C for 3 days. Transparent pale yellow prismatic crystals were formed. Yield of the reaction was ca. 40% based on TPPBDA ligand. Elemental analysis calcd. for C51H39N4O5Zn (1): C, 71.79; H, 4.61; N, 6.57, Found: C, 71.80; H, 4.68; N, 6.55. The IR spectra of the corresponding complex was shown in the Supporting Information ( |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
38% | In water; N,N-dimethyl-formamide at 90℃; for 72h; Autoclave; High pressure; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
10 mg | With tetrafluoroboric acid at 100℃; for 48h; High pressure; | 2.2. Synthesis and general characterizations Cu(TDBA)(DMA)2]·H2O (BUT-221). Cu(NO3)2·3H2O (12 mg, 0.07 mmol), H2TDBA (16 mg, 0.05 mmol), and one drop of HBF4 were ultrasonically dissolved in 2 mL of N,N-dimethylacetamide (DMA) in a 4 mL Pyrex vial.The mixture was then heated in a 100 °C oven for 48 h. After cooling to room temperature, the resulting blue crystals were harvested by filtration, washed with DMA and acetone, and then dried in air (yield: 10 mg).The PXRD, TGA, and FT-IR of the as-synthesized sample are provided in figures S1, S3, and S5. Elemental analysis (EA) for BUT-221, C24H21CuNO5 (446.5): Calcd C 46.50, H 4.70, N 3.14. Found. C 43.32, H 4.57, N 3.02. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
45% | With sodium hydroxide at 150℃; for 72h; High pressure; Autoclave; | Synthesis of [Ni2(dpb)(Hdpb)2(4,4′-bbibp)2(H2O)]·H2O}∞ mixture of H2dpb(0.20 mmol, 0.064 g), 4,4′-bbibp (0.20 mmol, 0.077 g), Ni(NO3)2·6H2O(0.20 mmol, 0.058 g), NaOH (0.40 mmol, 0.016 g) and 8 mL of water was placedin a Teflon-lined stainless steel vessel, heated to 150 °C for 3 days, and then cooled(a descent rate of 5 °C h-1) to room temperature. Green block crystals of 1 were obtained.Yield of 45% (based on Ni). Anal. (%) calcd. for C112H78Ni2N8O14: C, 71.66; H,4.19; N, 5.97. Found: C, 71.89; H, 4.21; N, 5.86. IR (KBr pellet, cm-1): 3393 (m),1700 (s), 1598 (s), 1450 (vs), 1356 (m), 765 (m), 676 (s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | With sodium hydroxide at 150℃; for 72h; High pressure; Autoclave; | Synthesis of [Ni2(dpb)(Hdpb)2(4,4′-bbibp)2(H2O)]·H2O}∞ General procedure: mixture of H2dpb(0.20 mmol, 0.064 g), 4,4′-bbibp (0.20 mmol, 0.077 g), Ni(NO3)2·6H2O(0.20 mmol, 0.058 g), NaOH (0.40 mmol, 0.016 g) and 8 mL of water was placedin a Teflon-lined stainless steel vessel, heated to 150 °C for 3 days, and then cooled(a descent rate of 5 °C h-1) to room temperature. Green block crystals of 1 were obtained.Yield of 45% (based on Ni). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | With sodium hydroxide at 150℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | In water; N,N-dimethyl-formamide at 120℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
60% | With sodium hydroxide at 150℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | In water; N,N-dimethyl-formamide at 120℃; for 72h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42% | With sodium hydroxide at 150℃; for 72h; High pressure; Autoclave; | 2.4 Synthesis of [Co2(tib)2(1,3-dpb)2]·H2O}n (3) A mixture of 1,3-H2dpb (0.20mmol, 0.064g), tib (0.20mmol, 0.056g), Co(NO3)2·6H2O (0.20mmol, 0.058g), NaOH (0.40mmol, 0.016g) and 8mL of water was placed in a Teflon-lined stainless steel vessel, heated to 150°C for 3days and then cooled (a descent rate of 5°Ch-1) to room temperature. Violet block crystals of 3 were obtained [5]. Yield of 42% (based on Co). Anal. (%) Calc. for C70H52Co2N12O10: C, 67.56; H, 4.18; N, 8.29. Found: C, 67.33; H, 4.26; N, 8.18. IR% (KBr pellet, cm-1): 3395 (w), 3142 (w), 1599 (s), 1547 (w), 1498 (s), 1384 (vs), 1237 (w), 1111 (w), 1065 (w), 1014 (w), 928 (w), 775 (m), 734 (w), 655 (w). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine at 85℃; for 12h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With triethylamine at 85℃; for 12h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
80% | With triethylamine at 85℃; for 12h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
42% | With sodium hydroxide; In water; at 160℃; for 72h;Autoclave; High pressure; | A mixture of H2dpb (0.20 mmol, 0.064 g), 4,40-<strong>[855766-92-6]bibp</strong> (0.20 mmol,0.058 g), MnCl24H2O (0.20 mmol, 0.040 g), NaOH (0.40 mmol,0.016 g) and 8 mL of water was placed in a Teflon-lined stainlesssteel vessel, heated to 160 C for 3 days, and then cooled (a descent rate of 5 C h-1) to room temperature. Colorless block crystals wereobtained. Yield of 42% (based on Mn). Anal. (%) calcd. ForC38H28MnN4O5: C, 67.56; H, 4.18; N, 8.29. Found: C, 67.12; H, 4.12; N,8.32. IR (KBr pellet, cm-1): 3295 (w), 3125 (m), 1605 (m), 1513 (m),1394 (vs), 1305 (w), 819 (w), 775 (m). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
81% | With acetic acid In N,N-dimethyl-formamide at 120℃; for 24h; Sealed tube; | Synthesis of [Zr6(μ3-O)4(μ3-OH)4(BDB)6] (BUT-66) In a 5mL glass vial, ZrOCl2·8H2O (0.0322 g, 0.1mmol) and H2BDB (0.0636 g, 0.2mmol) were added in a mixture of 1.5mL of N,N-dimethylformamide (DMF) and 0.25mL of acetic acid. The vial was then sealed and kept under ultrasonication for about 30min to dissolve all the starting materials. The mixture was heated at 120°C for 24hr and then cooled down to room temperature. Colorless hexagonal crystals were obtained by filtration. After the as-synthesized crystals were guest exchanged with methanol for 3days (20mL × 3) and subsequently evacuated at 80°C under high vacuum, 0.035g (yield ca. 81% based on Zr) of the final product of BUT-66 was obtained. Anal. calcd. (%) for C120H76O32Zr6: C, 55.92; H, 2.97. Found: C, 55.45; H, 3.06. FT-IR (KBr pellet, cm-1): 3412(m), 3068(w), 2927(w), 1662(s), 1583(s), 1412(s), 1257(m), 1153(w), 1087(w), 777(s), 653(s), 457(m) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
58% | With water; sodium hydroxide In methanol; butan-1-ol at 180℃; for 168h; Autoclave; | 2.2. Synthesis of 1 [Na2(DCPB)(H2O)2]n NaOH (0.10 mol L-1, 4 mL) and H2DCPB (0.031 mmol, 10mg) wereboth added into a Teflon-lined autoclave containing a mixed solution ofn-butyl alcohol (3.2 mL), H2O (0.2 mL), andMeOH (0.1 mL),whichwaskept under an ultrasound for 15 min at room temperature. The autoclavewas heated in an oven at 180 °C for one week. After cooling toroom temperature, well-shaped block crystals were generated andachieved. The final product was collected and dried in air with theyield of 58% (based on H2DCPB). Anal. Calcd for C20H16O6Na2: C,60.3%; H, 4.0%. Found: C, 59.9%; H, 4.1%. Selected FI-IR spectrum(cm-1, Fig. S1): 3459 (s), 3254 (s), 2186 (s), 1939 (s), 1676 (s), 1595(s), 1538 (s), 1407 (s), 1184 (s), 1106 (s), 1007 (s), 874 (s), 845 (s),777 (s), 710 (s), 545 (s), 459 (s). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | With acetic acid at 115℃; for 48h; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
17.19 mg | With N-formyldiethylamine; zinc(II) nitrate tetrahydrate at 100℃; for 24h; Sonication; |
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