2-Chloroethyl isocyanate → alpha-[N-(2-chloroethyl)ureido]benzylphosphonic acid diethyl ester

HRID 1285324노트

반응식

HRID 1285324 반응식
[CH2:1]([O:3][P:4]([CH:9](N)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[Cl:17][CH2:18][CH2:19][N:20]=[C:21]=[O:22].[NH2:23]P(=O)([O-])[O-]>C(Cl)(Cl)Cl>[CH2:6]([O:5][P:4]([CH:9]([N:20]([CH2:19][CH2:18][Cl:17])[C:21]([NH2:23])=[O:22])[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1)(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

참가 물질

5

반응물 3

HCID 160352-Chloroethyl isocyanateHCID 211207Phosphoramidic acid, ion(2-)HCID 419299Diethyl amino(phenyl)methylphosphonate

생성물 1

HCID 53798997alpha-[N-(2-chloroethyl)ureido]benzylphosphonic acid diethyl ester수율 85%

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
10 °C

실험 절차

A solution of 0.05 mol of α-aminobenzylphosphonic acid diethyl ester in 30 ml of chloroform is cooled to 0° C. in an ice-bath and then a large excess (0.06 mol) of β-chloroethyl isocyanate is added. The temperature of the reaction is then maintained at 10° C. while continuing stirring until the reaction is complete. (Examination by thin layer chromatography is used to ascertain that the starting aminophosphonate has disappeared completely. After evaporation of the solvent under reduced pressure, the crystalline residue is taken up in ether and filtered, yielding 14.8 g of crystals. Yield: 85%; m.p.=82° C.

후처리

  1. customAfter evaporation of the solvent under reduced pressure
  2. filtrationfiltered

출처 및 근거

ORD 기록
ord-0cf852b59ea6435d8966c57c256c5a66
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04567169

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