Pyridine → Ethyl (chlorosulfenyl)(1-methylethyl)carbamate

HRID 232723

반응식

HRID 232723 반응식
[CH3:1][CH:2]([NH:4][C:5](=[O:9])[O:6][CH2:7][CH3:8])[CH3:3].[S:10](Cl)[Cl:11].N1C=CC=CC=1>C(Cl)Cl>[Cl:11][S:10][N:4]([CH:2]([CH3:3])[CH3:1])[C:5](=[O:9])[O:6][CH2:7][CH3:8]

참가 물질

5

반응물 3

HCID 1049Pyridine2회HCID 17433Ethyl isopropylcarbamateHCID 25353Sulfur dichloride

생성물 1

HCID 20139494Ethyl (chlorosulfenyl)(1-methylethyl)carbamate수율 63.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

To a solution of ethyl (1-methylethyl)carbamate (13.1 g, 0.1 mol) in 100 ml methylene chloride cooled to 0° C. was added sulfur dichloride (11.3 g, 0.11 mol) in one portion. While maintaining the temperature of the mixture at 0° C., pyridine (8.7 g, 0.11 mol) was added dropwise over eleven minutes. After complete addition of the pyridine the temperature was allowed to rise to room temperature and stirring was continued for additional 1.5 hours. The mixture was let stand overnight. Methylene chloride was evaporated under vacuum and 100 ml hexane was added. Filteration of the pyridine hydrochloride and evaporation of hexane resulted in an orange oil which was distilled in a Kugelrohr apparatus to give 12.5 g of the title compound Bp: 64°-80° (bath temperature) at 1.4 mm Hg.

후처리

  1. customto rise to room temperature
  2. waitThe mixture was let stand overnight
  3. customMethylene chloride was evaporated under vacuum and 100 ml hexane
  4. additionwas added
  5. customFilteration of the pyridine hydrochloride and evaporation of hexane
  6. customresulted in an orange oil which
  7. distillationwas distilled in a Kugelrohr apparatus

출처 및 근거

ORD 기록
ord-2a23b4242a5f4f5f9d5abfbbd60b95d4
출처 데이터셋
uspto-grants-1997_01
특허 번호
US05591764

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