Acryloyl chloride → 3-(Acryloylmethylamino)benzoic Acid Methyl Ester

HRID 1055332노트

반응식

HRID 1055332 반응식
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH3:11])[CH:5]=1.C(=O)(O)[O-].[Na+].[C:18](Cl)(=[O:21])[CH:19]=[CH2:20]>C(Cl)Cl>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([NH:10][CH2:11][C:18](=[O:21])[CH:19]=[CH2:20])[CH:5]=1

참가 물질

5

반응물 3

HCID 13140Acryloyl chlorideHCID 516892Sodium Bicarbonate2회HCID 10899041Benzoic acid, 3-(methylamino)-, methyl ester

생성물 1

HCID 667703313-(Acryloylmethylamino)benzoic Acid Methyl Ester수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a stirred mixture of 3-methylaminobenzoic acid methyl ester (3.11 g, 18.8 mmol) and sodium bicarbonate (3.16 g, 37.6 mmol) in DCM (20.0 mL) at 0° C. was added 2-propenoyl chloride (2.29 mL, 28.2 mmol). The reaction mixture was stirred overnight at room temperature. Saturated aqueous sodium bicarbonate solution was added and the layers were separated. The organic layer was dried over sodium sulfate, filtered and concentrated under reduced pressure to give the title compound (4.12 g, 100% yield), which was used in the next reaction without further purification.

후처리

  1. customthe layers were separated
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-f8c5ac4827f941e988bad67fbbe7f0ed
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09394275B2

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