Sodium Bicarbonate → HCID 23333616、化合物

HRID 904182ノート

反応式

HRID 904182 の反応式
[CH3:1][NH:2][C:3]1[CH:8]=[CH:7][C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:5][CH:4]=1.C(=O)([O-])O.[Na+].Br[CH2:21][C:22]1[CH:32]=[CH:31][CH:30]=[CH:29][C:23]=1[C:24]([O:26][CH2:27][CH3:28])=[O:25]>O>[CH3:1][N:2]([CH2:21][C:22]1[CH:32]=[CH:31][CH:30]=[CH:29][C:23]=1[C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:3]1[CH:4]=[CH:5][C:6]([CH2:9][C:10]([O:12][CH2:13][CH3:14])=[O:11])=[CH:7][CH:8]=1

参加物

5

反応物 3

HCID 516892Sodium BicarbonateHCID 11032082Ethyl 2-(bromomethyl)benzoateHCID 11550151N-methyl-4-ethoxycarbonylmethylaniline

生成物 1

HCID 23333616HCID 23333616、化合物収率 112.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
90 °C

実験手順

A mixture of N-methyl-4-ethoxycarbonylmethylaniline (10 g), sodium hydrogencarbonate (5 g) and water (5 ml) was heated to 90° C. on an oil bath. Ethyl 2-bromomethylbenzoate (12.2 g) was gradually added dropwise to the mixture with stirring. Then, the mixture was stirred for 2 hours at 90° C. The reaction mixture was cooled, and extracted with benzene. The extract was washed with water. The benzene layer was extracted with 2 N-HCl. The aqueous layer was neutralized with potassium carbonate while cooling the layer with ice, and extracted with benzene. The benzene layer was dried over anhydrous magnesium sulfate. When the solvent was distilled off under reduced pressure, 20 g of N-methyl-N(2-ethoxycarbonylbenzyl)-4-ethoxycarbonylmethylaniline was obtained as a light-yellow oily material.

後処理

  1. stirringThen, the mixture was stirred for 2 hours at 90° C
  2. temperatureThe reaction mixture was cooled
  3. extractionextracted with benzene
  4. washThe extract was washed with water
  5. extractionThe benzene layer was extracted with 2 N-HCl
  6. temperaturewhile cooling the layer with ice
  7. extractionextracted with benzene
  8. dry with materialThe benzene layer was dried over anhydrous magnesium sulfate
  9. distillationWhen the solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-4d00114f1fd645269cc02d5db5861252
出典データセット
uspto-grants-1980_10
特許番号
US04230703

反応ノート

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