Octane → Phosphoramidic dichloride, bis(2-chloroethyl)-

HRID 267593

反応式

HRID 267593 の反応式
Cl.[Cl:2][CH2:3][CH2:4][NH:5][CH2:6][CH2:7][Cl:8].[P:9](Cl)([Cl:12])([Cl:11])=[O:10].NC1C=CC(S(C=CC#N)(=O)=O)=CC=1.CCCCCCCC>CC(C)=O.N1C=CC=CC=1>[Cl:2][CH2:3][CH2:4][N:5]([CH2:6][CH2:7][Cl:8])[P:9]([Cl:12])([Cl:11])=[O:10]

参加物

7

反応物 4

HCID 356OctaneHCID 24813Phosphorus oxychlorideHCID 522769Bis(2-chloroethyl)amine hydrochlorideHCID 545613262-Cyanovinyl 4-aminophenyl sulfone

生成物 1

HCID 96271Phosphoramidic dichloride, bis(2-chloroethyl)-

試薬・触媒・溶媒 2

HCID 180Acetone溶媒3 回HCID 1049Pyridine溶媒

実験手順

Di-(2-chloroethyl)amidophosphorodichloridate is prepared according to H. Brintzinger et al in Chemische Berichte 82, 389-99 (1949) from bis-(2-chloroethyl)amine hydrochloride and phosphoryl chloride in the presence of pyridine. 0.03 mol (7.8 g) of this material is dissolved in 100 ml of acetone and added to an acetone solution of 0.03 mole (6.3 g) of 2-cyanovinyl 4-aminophenyl sulfone. To the stirred mixture is added in 2-3 portions a 10% solution of 1,4-diazabicyclo[2.2.2.]octane in acetone. After a few minutes a yellow slurry forms which is stirred at room temperature for 30 minutes. After filtration to remove the amine hydrochlorides the filtrate is reduced to about half its volume by evaporation and then mixed with chloroform, washed with water and worked up. The light yellow solid is di-(2-chloroethyl)amido-di-4-(2-cyanoethenesulfonylanilido)phosphine oxide: ##SPC57##

後処理

  1. filtrationAfter filtration
  2. customto remove the amine hydrochlorides the filtrate
  3. customis reduced to about half its volume by evaporation
  4. additionmixed with chloroform
  5. washwashed with water

出典と根拠

ORDレコード
ord-985e4505f57f40b8bce98de6f210dac8
出典データセット
uspto-grants-1976_03
特許番号
US03943154

関連ノート

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