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Thiophosgene → Thiourea, N,N'-didodecyl-

HRID 867450
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HRID 867450 반응식
[C:1](Cl)(Cl)=[S:2].[CH2:5]([NH2:17])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]>C1(C)C=CC=CC=1>[CH2:5]([NH:17][C:1]([NH:17][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16])=[S:2])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 10040ThiophosgeneHCID 13583Dodecylamine

생성물 1

HCID 3034200Thiourea, N,N'-didodecyl-수율 75.5%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

Thiophosgene (10.0 mls, 0.13 moles) is added dropwise to a stirred solution of dodecylamine (100 g, 0.54 moles) in toluene (210 mls). The mixture is heated to reflux for four hours then cooled in an icebath. The precipitate is filtered off, rinsed with toluene then ether, and dried, then treated with hot dilute HCl, rinsed with water and redried. Recrystallization from ethyl acetate gave the product (40.5 g), mp 75°-78° C.

후처리

  • temperatureThe mixture is heated
  • temperatureto reflux for four hours
  • temperaturethen cooled in an icebath
  • filtrationThe precipitate is filtered off
  • washrinsed with toluene
  • dry with materialether, and dried
  • additiontreated with hot dilute HCl
  • washrinsed with water
  • customredried
  • customRecrystallization from ethyl acetate
  • 출처 및 근거

    ORD 기록
    ord-29fb0190e84f49ad91a2acf43365348d
    출처 데이터셋
    uspto-grants-1988_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04775677

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