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Ethyl chloroacetate → HCID 53739137、化合物

HRID 1164531
ノート
印刷プレビュー

反応式

HRID 1164531 の反応式
[O:1]=[C:2]1[CH2:10][C:9]2[C:4](=[CH:5][C:6]([Cl:12])=[C:7]([NH2:11])[CH:8]=2)[NH:3]1.C(=O)([O-])[O-].[K+].[K+].Cl[CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22]>CC(C)=O>[O:1]=[C:2]1[CH2:10][C:9]2[C:4](=[CH:5][C:6]([Cl:12])=[C:7]([NH2:11])[CH:8]=2)[N:3]1[CH2:20][C:21]([O:23][CH2:24][CH3:25])=[O:22]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 204666645-amino-6-chloro-2,3-dihydro-1H-indol-2-one

生成物 1

HCID 53739137HCID 53739137、化合物収率 19.1%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a mixture of 2-oxo-5-amino-6-chloroindoline (3.2 g), potassium carbonate (4.8 g) and acetone (60 ml) was added dropwise ethyl chloroacetate (3.2 g) at ambient temperature. The reaction mixture was refluxed with stirring for 4 hours and then filtered under warm condition. The filter cake was washed with acetone. The combined filtrate and washings were concentrated under reduced pressure to give a residue, which was purified by a column chromatography on silica gel to give crystalline ethyl 2-oxo-5-amino-6-chloro-1-indolineacetate (0.9 g).

後処理

  1. temperatureThe reaction mixture was refluxed
  2. filtrationfiltered
  3. temperatureunder warm condition
  4. washThe filter cake was washed with acetone
  5. concentrationThe combined filtrate and washings were concentrated under reduced pressure
  6. customto give a residue, which
  7. customwas purified by a column chromatography on silica gel

出典と根拠

ORDレコード
ord-e2fa5a2c04444ddf9ab904d5f9e53a1d
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04370340

反応ノート

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