N-(2,6-Dichlorophenyl)thiourea → 1,3-Dichloro-2-isothiocyanatobenzene
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
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
- concentrationconcentrated
- customThe resulting oil was triturated with 1 l
- filtrationof hot hexane which was filtered
- temperatureOn cooling overnight
- custom(36%) of 2,6-dichlorophenylisothiocyanate, m.p. 41°-42° separated
- customConcentration of the filtrate gave an additional 64.2 g
- customRecrystallization of a sample from hexane
- customgave the analytical sample, m.p. 41°-42°
出典と根拠
- ORDレコード
- ord-04cb315532594327a17fb16c2b3b836e
- 出典データセット
- uspto-grants-1979_04
- 特許番号
- US04150138
反応ノート
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