Water → 4-Bromomethyl benzoic acid 2,2,2-trichloroethyl ester

HRID 1172278

反応式

HRID 1172278 の反応式
[Cl:1][C:2]([Cl:6])([Cl:5])[CH2:3][OH:4].CCN(CC)CC.[Br:14][CH2:15][C:16]1[CH:24]=[CH:23][C:19]([C:20](Br)=[O:21])=[CH:18][CH:17]=1.O>C(Cl)Cl>[Cl:1][C:2]([Cl:6])([Cl:5])[CH2:3][O:4][C:20](=[O:21])[C:19]1[CH:23]=[CH:24][C:16]([CH2:15][Br:14])=[CH:17][CH:18]=1

参加物

6

反応物 4

HCID 962WaterHCID 8259TrichloroethanolHCID 8471TriethylamineHCID 46406714-Bromomethyl benzoyl bromide

生成物 1

HCID 117918784-Bromomethyl benzoic acid 2,2,2-trichloroethyl ester

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of 2,2,2-trichloroethanol (2.46 g, 16.5 mmol) and NEt3 (1.67 g, 16.5 mmol) in CH2Cl2 (40 ml) at 0° C. was dropwise added 4-bromomethyl benzoylbromide (4.17 g, 15.0 mmol) in CH2Cl2 (20 ml) and stirred to room temperature overnight. The reaction mixture was added H2O (20 ml) and the organic layer separated. The organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml). The organic layer was dried over Na2SO4, filtered and the solvent evaporated in vacuo to leave the expected product as a white solid. The product was used directly in the next step without any further purification (to be filled in).

後処理

  1. customat 0° C.
  2. customthe organic layer separated
  3. washThe organic layer washed with aqueous 1 M HCl (20 ml) and H2O (20 ml)
  4. dry with materialThe organic layer was dried over Na2SO4
  5. filtrationfiltered
  6. customthe solvent evaporated in vacuo

出典と根拠

ORDレコード
ord-61d2cf5a3ccc4acfb442a0fe0841cccd
出典データセット
uspto-grants-2010_11
特許番号
US07834010B2

関連ノート

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