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

HRID 236922

반응식

HRID 236922 반응식
[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]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 3120DiuronHCID 25353Sulfur dichloride

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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: %S, calc. 10.7, found 10.7; %Cl, calc. 35.6, found 35.4; %C, calc. 36.1, found 36.4; %H, calc. 3.0, found 3.2; %N, calc. 9.3, found 8.7.

후처리

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

출처 및 근거

ORD 기록
ord-b1cbc0777acb4a53bac295548b56241b
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04159281

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