Chloroacetyl chloride → HCID 57742180, 화합물

HRID 660286노트

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HRID 660286 반응식
[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]

참가 물질

5

반응물 2

HCID 6577Chloroacetyl chlorideHCID 12370790HCID 12370790, 화합물

생성물 1

HCID 57742180HCID 57742180, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 7909Methyl Isobutyl Ketone용매2회

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6d9ba94bba024f6fba3cf9061514cd10
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08084484B2

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