Pyridine → methyl 2-(dimethylamino)-N-[[[[[(diethoxyphosphinothioyl)methylamino]sulfinyl]methylamino]carbonyl]oxy]-2-oxoethanimidothioate

HRID 647795

반응식

HRID 647795 반응식
[CH3:1][N:2]([CH3:14])[C:3](=[O:13])[C:4]([S:11][CH3:12])=[N:5][O:6][C:7]([NH:9][CH3:10])=[O:8].[S:15](Cl)(Cl)=[O:16].CN[P:21](=[S:28])([O:25][CH2:26][CH3:27])[O:22][CH2:23][CH3:24].[N:29]1C=CC=C[CH:30]=1>>[CH3:14][N:2]([CH3:1])[C:3](=[O:13])[C:4]([S:11][CH3:12])=[N:5][O:6][C:7]([NH:9][CH2:10][S:15]([NH:29][CH2:30][P:21]([O:22][CH2:23][CH3:24])([O:25][CH2:26][CH3:27])=[S:28])=[O:16])=[O:8]

참가 물질

5

반응물 4

HCID 1049PyridineHCID 24386Thionyl ChlorideHCID 31657OxamylHCID 759370O,O-diethyl methylamidothiophosphate

생성물 1

HCID 86739080methyl 2-(dimethylamino)-N-[[[[[(diethoxyphosphinothioyl)methylamino]sulfinyl]methylamino]carbonyl]oxy]-2-oxoethanimidothioate

실험 절차

To a solution of methyl 2-(dimethylamino)-N-[[(methylamino)carbonyl]oxy]-2-oxoethanimidothioate (3.29 g, 0.015 mole) in dry pyridine 15 ml was added at one time thionyl chloride (1.79 g, 0.015 mole) at -30°. The mixture was allowed to come to room temperature and then stirred for 15 minutes. The mixture was cooled to 0° and O,O-diethyl methylphosphoramidothioate (2.75 g, 0.01 mole) was added. The mixture was allowed to come to room temperature for 1 hour, poured into ice water and extracted with benzene. The benzene solution was washed with water 4 times and then dried over anhydrous sodium sulfate. The benzene was removed under reduced pressure to give a crude product of the formula below. ##STR40##

후처리

  1. customto come to room temperature
  2. temperatureThe mixture was cooled to 0°
  3. waitto come to room temperature for 1 hour
  4. extractionextracted with benzene
  5. washThe benzene solution was washed with water 4 times
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe benzene was removed under reduced pressure

출처 및 근거

ORD 기록
ord-6055ec27227a4f8eb0e6bdafe6327d36
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04410518

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