Methanol → HCID 20577071, 화합물

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[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([F:14])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].O=S(Cl)Cl.[CH3:19]O>>[Br:1][C:2]1[C:10]([N+:11]([O-:13])=[O:12])=[CH:9][C:8]([F:14])=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]

참가 물질

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HCID 887Methanol

HCID 24386Thionyl Chloride

HCID 185485832-Bromo-5-fluoro-3-nitrobenzoic acid

생성물 1

HCID 20577071HCID 20577071, 화합물수율 84%

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온도: 65 °C

실험 절차

To the solution of 2-bromo-5-fluoro-3-nitrobenzoic acid (35 g) in MeOH (400 mL) was added SOCl2 (40 mL) drop-wise at 10-15° C. The reaction was then stirred at 65° C. for 1 h. After cooling to room temperature, the solvent was evaporated in vacuum to afford a residue, which was chromatographed on silica gel using gradient eluant of 0-100% EtOAc in hexane to provide methyl 2-bromo-5-fluoro-3-nitrobenzoate (20 g, 84%).

후처리

temperatureAfter cooling to room temperature
customthe solvent was evaporated in vacuum
customto afford a residue, which
customwas chromatographed on silica gel using gradient eluant of 0-100% EtOAc in hexane

출처 및 근거

ORD 기록: ord-67a2b8a66da548e8acde762fba7b729a
출처 데이터셋: uspto-grants-2016_05
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US09328111B2

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