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CAS No. : | 2973-78-6 | MDL No. : | MFCD00017348 |
Formula : | C7H5BrO2 | Boiling Point : | No data available |
Linear Structure Formula : | HOC6H3(Br)CHO | InChI Key : | UOTMHAOCAJROQF-UHFFFAOYSA-N |
M.W : | 201.02 | Pubchem ID : | 76308 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
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* 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 |
---|---|---|
35% | With di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at 20℃; for 20h;Cooling with ice; | To the ice-cooled solution of 3-bromo-4-hydroxybenzaldehyde 10 (0.71 g, 3.51 mmol) , triphenylphosphine (1.02 g, 3.89 mmol) and compound 4 (0.70 g, 0.52 mmol) in dry THF (21 mL) , diisopropyl azodicarboxylate (DIAD) (0.735 mL, 3.89 mmol) in THF (21 mL) was added dropwise. The resulting yellow solution was allowed to warm to room temperature and was stirred for additional 20 h. The mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel using 0-60% ethyl acetate in hexane . Recrystallization from MeOH yielded colourless solid (0.47 g, yield: 35%) .mp: 108.0-110.0 C; 1H NMR (600MHz, DMSO-d6) delta[ ppm]: 9.87 (s, 1H) , 8.14 (d, J=2.0 Hz, 1H) , 7.97 (dd, Jl= 6.5 Hz, J2=2.0 Hz, 1H) , 7.54 (m, 2H) , 7.46 (m, 2H) , 7.39 (m, 1H) , 7.33-7, 30 (m, 3H) , 7.22 (dd, Jl= 6.5 Hz, J2= 1 Hz, 1H) , 5.39 (s, 2H) , 2.23 (s, 3H) ; 13C NMR (151MHz, DMSO-d6) delta [ppm]: 190.6, 159.2, 142.2, 141.2, 134.6, 134.0, 133.9, 131.2, 130.8, 129.8, 129.2, 128.3, 127.5, 127.0, 125.6, 114.1, 111.9, 69.8, 15.9; IR V (ATR cm-1) 3063, 2852, 1689, 1594, 1278, 1254, 1189, 1048; HRMS (ESI-TOF) Calcd C21H17Br02 [M+Na]+: 403.0310; found [M+Na]+: 403.0302. |
106.9 mg | With di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at 0 - 20℃; | To a cooled (0C) solution of 3-bromo-4-hydroxybenzaldehyde (101 mg, 0.5 mmol), triphenylphosphine (146 mg, 0.555 mmol) and (2-methyl-[l,l'-biphenyl]-3- yl)methanol (100 mg, 0.504 mmol) in dry THF (3 mL) was added dropwise of diisopropyl azodicarboxylate (0.108 mL, 0.555 mmol) in THF (3 mL). The resulting yellow solution was allowed to slowly warm to room temperature while stirring overnight. Excess solvent was evaporated by rotary evaporation. The crude residue was dissolved in methanol and purified via preparative LC/MS with the following conditions: Column: Waters XBridge CI 8, 19 x 200 mm, 5-muiotaeta particles; Guard Column: Waters XBridge CI 8, 19 x 10 mm, 5-muiotaeta particles; Mobile Phase A: water with 20-mM ammonium acetate; Mobile Phase B: 95:5 acetonitrile: water with 20-mM ammonium acetate; Gradient: 30-100% B over 20 minutes, then a 4-minute hold at 100% B; Flow: 20 mL/min. Fractions containing the desired product were combined and dried via centrifugal evaporation. The yield of the product was 106.9 mg, and its estimated purity by LCMS analysis was 100%. LC/MS Method A: 3.1 minutes, M+1= 381.0, EM = 380.0. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
26% | With hydrogenchloride; acetic acid; In water; at 60℃; for 72h; | For the synthesis of compound g (MHY1498, (Z)-3-(3-bromo-4-hydroxybenzylidene)thiochroman-4-one), a solution of 3-bromo-4-hydroxybenzaldehyde (100 mg, 0.50 mmol) and thiochroman-4-one(53 L, 0.40 mmol) in 1.0MHCl acetic acid (0.5 mL) and 12.0M hydrochloric acid (0.02 mL) was heatedat 60 C for three days. The reaction mixture was divided between dichloromethane and water, and the organic layer was dried over anhydrous MgSO4, filtered, and evaporated in vacuo. The resultant residue was recrystallized in methanol and water to give MHY1498 (35.9 mg, 26%) as a yellow solid. |
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