Hydrochloric Acid → Ethyl (4-chlorobenzyl)carbamate

HRID 495625

반응식

HRID 495625 반응식
[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

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10928Ethyl chloroformateHCID 660364-Chlorobenzylamine

생성물 1

HCID 874364Ethyl (4-chlorobenzyl)carbamate수율 98%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-8537c4556af84daa82eae7dfe7af07d9
출처 데이터셋
uspto-grants-2005_09
특허 번호
US06939887B2

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