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Ethyl bromoacetate → ethyl 3,5-diethyl-1H-pyrazole-1-acetate

HRID 2043750
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HRID 2043750 반응식
[CH2:1]([C:3]1[CH2:7][C:6]([CH2:8][CH3:9])=[N:5][N:4]=1)[CH3:2].C(C1C=C(CC)NN=1)C.C(=O)([O-])[O-].[K+].[K+].Br[CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28]>CN(C)C=O>[CH2:1]([C:3]1[CH:7]=[C:6]([CH2:8][CH3:9])[N:5]([CH2:26][C:27]([O:29][CH2:30][CH3:31])=[O:28])[N:4]=1)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 43063673,5-diethyl-1H-pyrazoleHCID 588905493,5-diethyl-4H-pyrazole

생성물 1

HCID 67458757ethyl 3,5-diethyl-1H-pyrazole-1-acetate수율 77.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

To a solution of 3,5-diethyl-4H-pyrazole (2.14 g, 17.2 mmol) (i.e. the product of Example 15, Step A) in N,N-dimethylformamide (10 mL) was added potassium carbonate (4.7 g) and ethyl bromoacetate (2.9 mL, 26.1 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 reaction mixture was concentrated under reduced pressure to give 2.79 g of the title compound.

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 reaction mixture was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c5299b6f51fa4d7dbec6aa7a94348034
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08586611B2

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