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1,2-Dichloroethane → ethyl N-n-propoxycarbamate

HRID 1451192
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HRID 1451192 반응식
[CH2:1]([O:4][NH2:5])[CH2:2][CH3:3].C(Cl)CCl.C(=O)([O-])[O-].[K+].[K+].Cl[C:17]([O:19][CH2:20][CH3:21])=[O:18]>O>[CH2:1]([O:4][NH:5][C:17](=[O:18])[O:19][CH2:20][CH3:21])[CH2:2][CH3:3]
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참가 물질

6

반응물 4

HCID 111,2-DichloroethaneHCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 2768918O-propylhydroxylamine

생성물 1

HCID 21475744ethyl N-n-propoxycarbamate수율 93.6%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

22 g (197 mmol) of n-propoxyamine hydroxhloride was dissolved in 100 ml of water, and 200 ml of ethylene dichloride was added thereto. Then, 27.2 g (197 mmol) of potassium carbonate was added in several times under cooling, and then 21.3 g (196 mmol) of ethyl chloroformate was dropwise added thereto at a temperature of not higher than 10° C. After raising the temperature to room temperature, the mixture was further stirred at the same temperature for 4 hours. The ethylene dichloride layer was separated, and then the aqueous layer was extracted twice with 100 ml of chloroform. The ethylene dichloride layer and the chloroform layer were put together, and washed with a saturated sodium chloride aqueous solution, and then dried over anhydrous sodium sulfate. Then, the solvent was distilled off under reduced pressure. 27 g of ethyl N-n-propoxycarbamate was obtained by distillation under reduced pressure. Boiling point: 88° C./2.5 mmHg

후처리

  1. temperatureunder cooling
  2. customhigher than 10° C
  3. customThe ethylene dichloride layer was separated
  4. extractionthe aqueous layer was extracted twice with 100 ml of chloroform
  5. washwashed with a saturated sodium chloride aqueous solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThen, the solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-461cc35615614caa943066bac2505bf4
출처 데이터셋
uspto-grants-1997_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05604179

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