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

HRID 1055332ノート

反応式

HRID 1055332 の反応式
[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

参加物

5

反応物 3

HCID 13140Acryloyl chlorideHCID 516892Sodium Bicarbonate2 回HCID 10899041Benzoic acid, 3-(methylamino)-, methyl ester

生成物 1

HCID 667703313-(Acryloylmethylamino)benzoic Acid Methyl Ester収率 100%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-f8c5ac4827f941e988bad67fbbe7f0ed
出典データセット
uspto-grants-2016_07
特許番号
US09394275B2

反応ノート

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