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

HRID 1172278

반응식

HRID 1172278 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-61d2cf5a3ccc4acfb442a0fe0841cccd
출처 데이터셋
uspto-grants-2010_11
특허 번호
US07834010B2

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