Methanol → Methyl 4-bromo-2,5-difluorobenzoate

HRID 452461

反応式

HRID 452461 の反応式
[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([F:12])[CH:3]=1.[CH3:13]O>>[Br:1][C:2]1[C:10]([F:11])=[CH:9][C:5]([C:6]([O:8][CH3:13])=[O:7])=[C:4]([F:12])[CH:3]=1

参加物

3

反応物 2

HCID 887MethanolHCID 8228574-Bromo-2,5-difluorobenzoic acid

生成物 1

HCID 66887346Methyl 4-bromo-2,5-difluorobenzoate

実験手順

4-bromo-2,5-difluorobenzoic acid (4.82 g, 20.3 mmol) and methanol (100 ml, saturated with gaseous HCl) was heated at 65° C. for 3 h. The volatiles were evaporated, MeOH was added and once again it was evaporated. This procedure was repeated three times. Purification by flash column chromatography (isooctane/EtOAc 4:1) gave the title compound (4.2 g). MS m/z (rel. intensity, 70 eV) 252 (M+, 33), 250 (M+, 34), 221 (95), 219 (bp), 193 (20), 191 (21), 112 (32).

後処理

  1. customThe volatiles were evaporated
  2. additionMeOH was added
  3. customonce again it was evaporated
  4. customPurification by flash column chromatography (isooctane/EtOAc 4:1)

出典と根拠

ORDレコード
ord-e7d8122d4d2541f782692e9081313de3
出典データセット
uspto-grants-2013_07
特許番号
US08492372B2

関連ノート

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