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

HRID 1763881

反応式

HRID 1763881 の反応式
[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]

参加物

3

反応物 1

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

生成物 1

HCID 1232391,3-Dichloro-2-isothiocyanatobenzene

試薬・触媒・溶媒 1

HCID 7964Chlorobenzene溶媒

実験手順

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°.

後処理

  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°

出典と根拠

ORDレコード
ord-aa6661741d884f6a978e41912c62fe2e
出典データセット
uspto-grants-1978_09
特許番号
US04113776

関連ノート

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