Ethyl bromoacetate → ethyl 5-ethyl-3-(trifluoromethyl)-1H-pyrazole-1-acetate

HRID 2043754노트

반응식

HRID 2043754 반응식
[CH2:1]([C:3]1[NH:7][N:6]=[C:5]([C:8]([F:11])([F:10])[F:9])[CH:4]=1)[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21]>CN(C)C=O>[CH2:1]([C:3]1[N:7]([CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[N:6]=[C:5]([C:8]([F:10])([F:11])[F:9])[CH:4]=1)[CH3:2]

참가 물질

5

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 230062095-ethyl-3-(trifluoromethyl)-1H-pyrazole2회

생성물 1

HCID 67464244ethyl 5-ethyl-3-(trifluoromethyl)-1H-pyrazole-1-acetate수율 63%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 5-ethyl-3-(trifluoromethyl)-1H-pyrazole (1.39 g, 8.5 mmol) (i.e. the product of Example 16, Step A) in N,N-dimethylformamide (10 mL) was added potassium carbonate (2.3 g) and ethyl bromoacetate (1.4 mL, 12.6 mmol). The reaction mixture was stirred at room temperature overnight. The resulting solids were filtered off and the filtrate was diluted with ethyl acetate, washed with water and dried over MgSO4. The resulting solution was concentrated under reduced pressure to give 1.34 g of the title compound. This compound was of sufficient purity to use in subsequent reactions.

후처리

  1. filtrationThe resulting solids were filtered off
  2. additionthe filtrate was diluted with ethyl acetate
  3. washwashed with water
  4. dry with materialdried over MgSO4
  5. concentrationThe resulting solution was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-9080a836df1240f8a3ceff46ce2c9b6b
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586611B2

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