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

HRID 2043739ノート

反応式

HRID 2043739 の反応式
[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

参加物

6

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 203280693,5-dichloro-1H-pyrazole2 回

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-dd47032d9e9d4578891876cca7350dcc
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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