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

HRID 1706707ノート

反応式

HRID 1706707 の反応式
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]

参加物

7

反応物 4

HCID 3283Diethyl Ether2 回HCID 9414MexacarbateHCID 61680MAGNESIUM SILICATE (synthetic)HCID 20333951O,O-diethyl N-(chlorothio)-n-propylphosphoramidothioate

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8058Hexane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-bd38786dba574ae688e17087aaf30751
出典データセット
uspto-grants-1980_06
特許番号
US04208409

反応ノート

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