Diethyl Ether → 4-(Dimethylamino)-3,5-xylyl [[(diethoxyphosphinothioyl)-n-propylamino]thio]methylcarbamate

HRID 1706707노트

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HRID 1706707 반응식
Cl[S:2][N:3]([CH2:12][CH2:13][CH3:14])[P:4](=[S:11])([O:8][CH2:9][CH3:10])[O:5][CH2:6][CH3:7].[CH3:15][NH:16][C:17](=[O:30])[O:18][C:19]1[CH:24]=[C:23]([CH3:25])[C:22]([N:26]([CH3:28])[CH3:27])=[C:21]([CH3:29])[CH:20]=1.[O-][Si]([O-])=O.[Mg+2].C(OCC)C>CN(C)C=O.CCCCCC>[CH2:6]([O:5][P:4]([N:3]([CH2:12][CH2:13][CH3:14])[S:2][CH2:15][NH:16][C:17](=[O:30])[O:18][C:19]1[CH:24]=[C:23]([CH3:25])[C:22]([N:26]([CH3:27])[CH3:28])=[C:21]([CH3:29])[CH:20]=1)([O:8][CH2:9][CH3:10])=[S:11])[CH3:7]

참가 물질

7

반응물 4

HCID 3283Diethyl Ether2회HCID 9414MexacarbateHCID 61680MAGNESIUM SILICATE (synthetic)HCID 20333951O,O-diethyl N-(chlorothio)-n-propylphosphoramidothioate

생성물 1

HCID 867370564-(Dimethylamino)-3,5-xylyl [[(diethoxyphosphinothioyl)-n-propylamino]thio]methylcarbamate

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8058Hexane용매

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온도
25 °C

실험 절차

The crude O,O-diethyl N-(chlorothio)-n-propylphosphoramidothioate (prepared in Preparation I) is cooled in an ice-bath and 2.79 gm. (0.013 mole) of 4-(dimethylamino)-3,5-xylyl methylcarbamate dissolved in 20 ml dimethylformamide (with 2 ml triethylamine added) are mixed as a batch. This reaction mixture is stirred at 25° C. for four hours, and then diluted with hexane. The organic solution is washed with water, dried over anhydrous sodium sulfate, and the organic solvents are removed by evaporation under reduced pressure. The residue thus obtained is transferred to a column of "Florisil". The chromatogram is developed first with a solvent mixture consisting of 10 percent diethyl ether in petroleum ether, and finally with 30 percent diethyl ether in petroleum ether. After collecting the later eluate and removing the solvents by evaporation under reduced pressure, there is obtained the desired 4-(dimethylamino)-3,5-xylyl [[(diethoxyphosphinothioyl)-n-propylamino]thio]methylcarbamate as a yellow oil.

후처리

  1. additionare mixed as a batch
  2. washThe organic solution is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. customthe organic solvents are removed by evaporation under reduced pressure
  5. customThe residue thus obtained
  6. customAfter collecting the later eluate
  7. customremoving the solvents
  8. customby evaporation under reduced pressure

출처 및 근거

ORD 기록
ord-bd38786dba574ae688e17087aaf30751
출처 데이터셋
uspto-grants-1980_06
특허 번호
US04208409

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