Pyridine → methyl N-[methyl(phenylsulfinothioyl)carbamoyl]oxyethanimidothioate

HRID 443924

반응식

HRID 443924 반응식
[CH3:1][NH:2][C:3]([O:5][N:6]=[C:7]([S:9][CH3:10])[CH3:8])=[O:4].N1C=CC=CC=1.[S:17](Cl)(Cl)=O.[C:21]1([SH:27])[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>O1CCCC1>[CH3:1][N:2]([S:27]([C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=[S:17])[C:3]([O:5][N:6]=[C:7]([S:9][CH3:10])[CH3:8])=[O:4]

참가 물질

6

반응물 4

HCID 1049Pyridine2회HCID 4109MethomylHCID 7969ThiophenolHCID 24386Thionyl Chloride

생성물 1

HCID 131712178methyl N-[methyl(phenylsulfinothioyl)carbamoyl]oxyethanimidothioate

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 3.3 g S-methyl N-[N'-methylcarbamoyloxy]thioacetimidate (0.02 mol), 1.9 g pyridine (0.024 mol) and 2.5 g thionyl chloride (0.021 mol), in 20 ml dry tetrahydrofuran was stirred at room temperature for 4 hours. Pyridine (1.9 g, 0.024 mol) was added and followed by 2.2 g benzenethiol (0.02 mol) added dropwise at water bath temperature. Stirring was continued for an additional hour, and the mixture was worked up as described for Example I. The resulting oily residue was purified by preparative thin-layer chromatography, and the NMR spectrum obtained.

후처리

  1. additionadded dropwise at water bath temperature
  2. waitwas continued for an additional hour
  3. customThe resulting oily residue was purified by preparative thin-layer chromatography
  4. customthe NMR spectrum obtained

출처 및 근거

ORD 기록
ord-0618ebcacf30466883b713ededabcaae
출처 데이터셋
uspto-grants-1981_04
특허 번호
US04262015

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