Pyridine → N-chlorothio-N-(3,4-dichlorophenyl)-N',N'-dimethyl urea

HRID 268106

反応式

HRID 268106 の反応式
[S:1]([Cl:3])Cl.[Cl:4][C:5]1[CH:6]=[C:7]([NH:12][C:13]([N:15]([CH3:17])[CH3:16])=[O:14])[CH:8]=[CH:9][C:10]=1[Cl:11].N1C=CC=CC=1>C(Cl)Cl>[Cl:3][S:1][N:12]([C:7]1[CH:8]=[CH:9][C:10]([Cl:11])=[C:5]([Cl:4])[CH:6]=1)[C:13]([N:15]([CH3:16])[CH3:17])=[O:14]

参加物

5

反応物 3

HCID 1049PyridineHCID 3120DiuronHCID 25353Sulfur dichloride

生成物 1

HCID 21314660N-chlorothio-N-(3,4-dichlorophenyl)-N',N'-dimethyl urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A 5.7-g (0.055 mol) sample of sulfur dichloride was added dropwise to a mixture of 11.7 g (0.05 mol) of N-(3,4-dichlorophenyl)-N',N'-dimethyl urea and 4.7 g (0.06 mol) pyridine in 50 ml methylene chloride cooled in an ice bath. After the completion of the addition, the pyridine hydrochloride was filtered. Hexane was added to precipitate additional pyridine hydrochloride, which was removed by filtration. Evaporation of the resulting filtrate gave the product as a clear yellow oil. The NMR spectrum showed an N',N'-dimethyl singlet at 3.0 ppm (relative to tetramethylsilane). Elemental analysis showed:

後処理

  1. temperaturecooled in an ice bath
  2. additionAfter the completion of the addition
  3. filtrationthe pyridine hydrochloride was filtered
  4. additionHexane was added
  5. customto precipitate additional pyridine hydrochloride, which
  6. customwas removed by filtration
  7. customEvaporation of the resulting filtrate

出典と根拠

ORDレコード
ord-d47b21a9c862486191a158b501967d1d
出典データセット
uspto-grants-1976_03
特許番号
US03946062

関連ノート

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