Methanol → Methyl 2,6-difluoro-4-hydroxybenzoate

HRID 82784노트

반응식

HRID 82784 반응식
O=S(Cl)Cl.[F:5][C:6]1[CH:14]=[C:13]([OH:15])[CH:12]=[C:11]([F:16])[C:7]=1[C:8]([OH:10])=[O:9].[CH3:17]O>>[F:5][C:6]1[CH:14]=[C:13]([OH:15])[CH:12]=[C:11]([F:16])[C:7]=1[C:8]([O:10][CH3:17])=[O:9]

참가 물질

4

반응물 3

HCID 887MethanolHCID 24386Thionyl ChlorideHCID 27787762,6-difluoro-4-Hydroxybenzoic Acid

생성물 1

HCID 22087431Methyl 2,6-difluoro-4-hydroxybenzoate수율 99%

실험 절차

SOCl2 (4.16 g, 30.1 mmol) was added to a solution of 2,6-difluoro-4-hydroxybenzoic acid (1.50 g, 8.62 mmol) in MeOH (20 mL) and the resulting mixture was heated at reflux for 24 h. After cooling the solvent was removed in vacuo to give the title compound (1.62 g, 99%) as a white crystalline solid; mp 177.5-180° C.; 1H NMR (270 MHz, DMSO-d6) 3.80 (3H, s, CH3), 6.50-6.60 (2H, m, ArH), 11.16 (1H, s, OH)

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 24 h
  3. temperatureAfter cooling the solvent
  4. customwas removed in vacuo

출처 및 근거

ORD 기록
ord-684f4c34193e42d59ba6b0a5c7b2c560
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846737B2

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