Chloroacetyl chloride → HCID 57742180、化合物

HRID 660286ノート

反応式

HRID 660286 の反応式
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][C:3]=1[OH:15].[Cl:16][CH2:17][C:18](Cl)=[O:19]>CC(C)CC(=O)C.O>[Cl:16][CH2:17][C:18]([NH:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([CH3:14])[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[CH:4][C:3]=1[OH:15])=[O:19]

参加物

5

反応物 2

HCID 6577Chloroacetyl chlorideHCID 12370790HCID 12370790、化合物

生成物 1

HCID 57742180HCID 57742180、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 7909Methyl Isobutyl Ketone溶媒2 回

反応条件

温度
80 °C

実験手順

A solution of Ethyl 2-(4-amino-3-hydroxyphenyl)propanoate (101 mg, 0.483 mmol) in 4-methyl-2-pentanone (4 mL) was added chloroacetyl chloride (58 mg, 0.514 mmol) in 4-methyl-2-pentanone (2 mL) at room temperature. The reaction mixture was stirred for 12 hrs at 80° C. then cooled to room temperature. The mixture was diluted with H2O and extracted with EtOAc. The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using EtOAc:hexanes (1:2) as eluant.

後処理

  1. temperaturethen cooled to room temperature
  2. extractionextracted with EtOAc
  3. dry with materialThe organic layer was dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified by flash column chromatography on silica gel

出典と根拠

ORDレコード
ord-6d9ba94bba024f6fba3cf9061514cd10
出典データセット
uspto-grants-2011_12
特許番号
US08084484B2

反応ノート

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