2-Chloroethanol → 2-Chloroethyl N-(2-chloro-4-nitrophenyl)carbamate

HRID 902998노트

반응식

HRID 902998 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[N:11]=[C:12]=[O:13].[Cl:14][CH2:15][CH2:16][OH:17].CCOCC>CCCCCC>[Cl:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[NH:11][C:12](=[O:13])[O:17][CH2:16][CH2:15][Cl:14]

참가 물질

5

반응물 3

HCID 342-ChloroethanolHCID 3283Diethyl EtherHCID 46142212-Chloro-4-nitrophenyl isocyanate

생성물 1

HCID 3107132-Chloroethyl N-(2-chloro-4-nitrophenyl)carbamate

시약·촉매·용매 1

HCID 8058Hexane용매

반응 조건

온도
15 °C

실험 절차

50.0 g of 2-chloro-4-nitrophenyl isocyanate was added, with stirring, to 100 g of 2-chloroethanol. After 2 minutes, the temperature of the mixture rose to 65° C. The mixture then was heated at 80°-90° C. for 10 minutes, and cooled. 200 ml of ether and 200 ml of hexane were added, the mixture was cooled to 15° C. and filtered. Drying of the filter cake gave 2-chloroethyl (2-chloro-4-nitrophenyl)carbamate (1A), as a white solid, mp: 128°-130° C.

후처리

  1. customrose to 65° C
  2. temperatureThe mixture then was heated at 80°-90° C. for 10 minutes
  3. temperaturecooled
  4. filtrationfiltered
  5. customDrying of the filter cake

출처 및 근거

ORD 기록
ord-58878eaa9ab94d928c8cef230751b479
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04226612

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