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

HRID 82784ノート

反応式

HRID 82784 の反応式
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]

参加物

4

反応物 3

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

生成物 1

HCID 22087431Methyl 2,6-difluoro-4-hydroxybenzoate収率 99%

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-684f4c34193e42d59ba6b0a5c7b2c560
出典データセット
uspto-grants-2014_09
特許番号
US08846737B2

反応ノート

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