Water → HCID 17934659、化合物

HRID 489227

反応式

HRID 489227 の反応式
[F:1][C:2]([F:15])([F:14])[S:3]([O:6]S(C(F)(F)F)(=O)=O)(=[O:5])=[O:4].O[C:17]1[CH:29]=[CH:28][C:20]([C:21]([O:23][C:24]([CH3:27])([CH3:26])[CH3:25])=[O:22])=[CH:19][CH:18]=1.O>C(Cl)Cl>[C:24]([O:23][C:21](=[O:22])[C:20]1[CH:28]=[CH:29][C:17]([O:6][S:3]([C:2]([F:15])([F:14])[F:1])(=[O:5])=[O:4])=[CH:18][CH:19]=1)([CH3:27])([CH3:25])[CH3:26]

参加物

5

反応物 3

HCID 962WaterHCID 67749Trifluoromethanesulfonic anhydrideHCID 117640tert-Butyl 4-hydroxybenzoate

生成物 1

HCID 17934659HCID 17934659、化合物収率 87.1%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Trifluoromethanesulfonic anhydride (1.04 ml, 6.2 mmol) was added to a cooled (5° C.) solution of tert-butyl 4-hydroxybenzoate (1 g, 5.1 mmol) in a mixture of DCM (25 ml) and TEA (1.1 ml, 7.8 mmol). After 4 h at 5° C., water was added. The organic layer was separated, dried over MgSO4 and concentrated in vacuo. The residue was chromatographed over silica gel (eluent: cyclohexane/iPr2O 95/5) to yield the above-titled compound as a colorless oil (1.45 g). 1H NMR (CDCl3): 8.09 (2H, d, J=8.6 Hz), 7.32 (2H, d, J=8.6 Hz), 1.60 (9H, s).

後処理

  1. customThe organic layer was separated
  2. dry with materialdried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was chromatographed over silica gel (eluent: cyclohexane/iPr2O 95/5)

出典と根拠

ORDレコード
ord-ba8d1a6d6ea141dfb286a494f23b81fe
出典データセット
uspto-grants-2005_12
特許番号
US06977267B2

関連ノート

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