Hydrochloric Acid → Ethyl (4-chlorobenzyl)carbamate

HRID 495625

反応式

HRID 495625 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1.Cl[C:11]([O:13][CH2:14][CH3:15])=[O:12].Cl>N1C=CC=CC=1>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH:7][C:11](=[O:12])[O:13][CH2:14][CH3:15])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 660364-Chlorobenzylamine

生成物 1

HCID 874364Ethyl (4-chlorobenzyl)carbamate収率 98%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

4-Chlorobenzylamine (1.0556 g) was dissolved in pyridine (5 ml), and to the solution was added dropwise ethyl chloroformate.(0.855 ml) during 5 minutes under ice-cooling. After the mixture was stirred for 3 hours, 1N hydrochloric acid was added and the mixture was extracted with ethyl acetate. The organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution, and then saturated brine, dried over anhydrous magnesium sulfate, and concentrated in vacuo to give the title compound (1.562 g, 98%).

後処理

  1. temperature(0.855 ml) during 5 minutes under ice-cooling
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution
  4. dry with materialsaturated brine, dried over anhydrous magnesium sulfate
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8537c4556af84daa82eae7dfe7af07d9
出典データセット
uspto-grants-2005_09
特許番号
US06939887B2

関連ノート

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