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

HRID 267593

반응식

HRID 267593 반응식
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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 180Acetone용매3회HCID 1049Pyridine용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-985e4505f57f40b8bce98de6f210dac8
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03943154

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