N-(2,6-Dichlorophenyl)thiourea → 1,3-Dichloro-2-isothiocyanatobenzene

HRID 26433

반응식

HRID 26433 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10](N)=[S:11]>ClC1C=CC=CC=1>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[N:9]=[C:10]=[S:11]

참가 물질

3

반응물 1

HCID 722776N-(2,6-Dichlorophenyl)thiourea

생성물 1

HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

시약·촉매·용매 1

HCID 7964Chlorobenzene용매

실험 절차

A solution of 156.9 g. of 1-(2,6-dichlorophenyl)thiourea in 1 l. of chlorobenzene was refluxed for 20 hours and concentrated. The resulting oil was triturated with 1 l. of hot hexane which was filtered. On cooling overnight, 52 g. (36%) of 2,6-dichlorophenylisothiocyanate, m.p. 41°-42° separated. Concentration of the filtrate gave an additional 64.2 g. (44%), m.p. 41°-43° in two crops. Recrystallization of a sample from hexane gave the analytical sample, m.p. 41°-42°.

후처리

  1. concentrationconcentrated
  2. customThe resulting oil was triturated with 1 l
  3. filtrationof hot hexane which was filtered
  4. temperatureOn cooling overnight
  5. custom(36%) of 2,6-dichlorophenylisothiocyanate, m.p. 41°-42° separated
  6. customConcentration of the filtrate gave an additional 64.2 g
  7. customRecrystallization of a sample from hexane
  8. customgave the analytical sample, m.p. 41°-42°

출처 및 근거

ORD 기록
ord-04cb315532594327a17fb16c2b3b836e
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04150138

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