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

HRID 2043754ノート

反応式

HRID 2043754 の反応式
[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]

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 230062095-ethyl-3-(trifluoromethyl)-1H-pyrazole2 回

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9080a836df1240f8a3ceff46ce2c9b6b
出典データセット
uspto-grants-2013_11
特許番号
US08586611B2

反応ノート

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