Sodium hydride → HCID 59713040, 화합물

HRID 2222753노트

반응식

HRID 2222753 반응식
[CH3:1][O:2][C:3](=[O:17])[CH:4]([C:6]1[CH:11]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:9]=[C:8]([F:16])[CH:7]=1)[OH:5].[H-].[Na+].[H][H].F[C:23]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:24]=1[C:30]([F:33])([F:32])[F:31]>CN(C)C=O.C(OCC)(=O)C.O>[CH3:1][O:2][C:3](=[O:17])[CH:4]([C:6]1[CH:11]=[C:10]([C:12]([F:14])([F:15])[F:13])[CH:9]=[C:8]([F:16])[CH:7]=1)[O:5][C:25]1[CH:26]=[C:27]([Cl:29])[CH:28]=[CH:23][C:24]=1[C:30]([F:31])([F:32])[F:33]

참가 물질

8

반응물 4

HCID 24758Sodium hydrideHCID 142277984-Chloro-2-fluoro-1-(trifluoromethyl)benzeneHCID 59713034HCID 59713034, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 59713040HCID 59713040, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매

실험 절차

(3-Fluoro-5-trifluoromethyl-phenyl)-hydroxy-acetic acid methyl ester 91 (0.1 mol) was dissolved in dimethylformamide (100 mL) and sodium hydride (0.1 mol) was added. When hydrogen evolution stopped, a solution of 2-fluoro-4-chloro-1-trifluoromethyl-benzene 92 (0.1 mol) in dimethylformamide (25 mL) was added. The progress of the reaction was monitored by TLC. When the reaction was complete, water and ethyl acetate were added. The organic phase was dried and concentrated, and the residue was chromatographed to afford (3-fluoro-5-trifluoromethyl-phenyl)-(5-chloro-2-trifluoromethyl-phenoxy)-acetic acid methyl ester 93. Basic hydrolysis of this compound, as described in Example 1, then afforded the title compound 94.

후처리

  1. customThe organic phase was dried
  2. concentrationconcentrated
  3. customthe residue was chromatographed

출처 및 근거

ORD 기록
ord-27a8879c3d184bbf9287c3da7578f548
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07371888B2

반응 노트

불러오는 중…