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

HRID 2043739노트

반응식

HRID 2043739 반응식
[Cl:1][C:2]1[CH:6]=[C:5]([Cl:7])[NH:4][N:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17]>CN(C)C=O.C(OCC)(=O)C>[Cl:1][C:2]1[CH:6]=[C:5]([Cl:7])[N:4]([CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])[N:3]=1

참가 물질

6

반응물 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 203280693,5-dichloro-1H-pyrazole2회

생성물 1

HCID 67463975ethyl 3,5-dichloro-1H-pyrazole-1-acetate수율 94.1%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

A suspension of 3,5-dichloro-1H-pyrazole (690 mg, 5.0 mmol) (i.e. the product of Example 12, Step D), potassium carbonate (3 g, 21 mmol) in N,N-dimethylformamide (10 mL) was treated with ethyl bromoacetate (1.0 mL, 9.0 mmol) and stirred at ambient temperature for 12 h. The suspension was diluted with ethyl acetate, washed with water, and dried over MgSO4. The reaction mixture was then concentrated under reduced pressure giving 1.05 g of the title compound. This compound was of sufficient purity to use in subsequent reactions.

후처리

  1. washwashed with water
  2. dry with materialdried over MgSO4
  3. concentrationThe reaction mixture was then concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-dd47032d9e9d4578891876cca7350dcc
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08586611B2

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