Potassium Carbonate → (((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methyl)thio)acetic acid, ethyl ester

HRID 1198426노트

반응식

HRID 1198426 반응식
Br[CH2:2][C:3]1[C:4]([Cl:21])=[CH:5][C:6]([F:20])=[C:7]([C:9]2[C:13]([Cl:14])=[C:12]([C:15]([F:18])([F:17])[F:16])[N:11]([CH3:19])[N:10]=2)[CH:8]=1.[SH:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25].C([O-])([O-])=O.[K+].[K+]>CC(C)=O>[Cl:21][C:4]1[CH:5]=[C:6]([F:20])[C:7]([C:9]2[C:13]([Cl:14])=[C:12]([C:15]([F:18])([F:17])[F:16])[N:11]([CH3:19])[N:10]=2)=[CH:8][C:3]=1[CH2:2][S:22][CH2:23][C:24]([O:26][CH2:27][CH3:28])=[O:25]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12185Ethyl ThioglycolateHCID 194367643-[5-(bromomethyl)-4-chloro-2-fluorophenyl]-4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazole

생성물 1

HCID 86747525(((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methyl)thio)acetic acid, ethyl ester수율 96%

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

A mixture of 1.62 g (4.0 mmole) 3-[5-(bromomethyl)-4-chloro-2-fluorophenyl]-4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazole, 0.44 mL ethyl mercaptoacetate and 0.55 g K2CO3 was slurried in 25 mL of acetone. The reaction mixture was allowed to stir at room temperature overnight. After dilution with 100 mL of cold water, the mixture was extracted with ethyl acetate, the organic extracts washed with water, dried with MgSO4 and concentrated in vacuo. The residue was purified by chromatography to afford 1.7 g (96%) of (((2-chloro-5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluorophenyl)methyl)thio)acetic acid, ethyl ester as a white solid; mp 63° C.

후처리

  1. extractionAfter dilution with 100 mL of cold water, the mixture was extracted with ethyl acetate
  2. washthe organic extracts washed with water
  3. dry with materialdried with MgSO4
  4. concentrationconcentrated in vacuo
  5. customThe residue was purified by chromatography

출처 및 근거

ORD 기록
ord-ff11e6cdea634303af0b58709b77f64f
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05281571

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