Diethyl Ether → N'-t-butyl-N'-[methyl-(2-chlorophenylamino)phosphinyl]-N-benzoylhydrazine

HRID 849799

반응식

HRID 849799 반응식
[CH3:1][P:2](Cl)Cl.[C:5]([NH:13][NH:14][C:15]([CH3:18])([CH3:17])[CH3:16])(=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1.[Cl:19][C:20]1[CH:26]=[CH:25][CH:24]=[CH:23][C:21]=1[NH2:22].CC[O:29]CC>C(N(CC)CC)C.C(Cl)Cl>[C:15]([N:14]([P:2]([CH3:1])([NH:22][C:21]1[CH:23]=[CH:24][CH:25]=[CH:26][C:20]=1[Cl:19])=[O:29])[NH:13][C:5](=[O:12])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)([CH3:18])([CH3:17])[CH3:16]

참가 물질

7

반응물 4

HCID 3283Diethyl EtherHCID 72402-ChloroanilineHCID 61194Methyl phosphonous dichlorideHCID 299436N'-tert-butylbenzohydrazide

생성물 1

HCID 19368069N'-t-butyl-N'-[methyl-(2-chlorophenylamino)phosphinyl]-N-benzoylhydrazine

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

Methyl dichlorophosphine (1.3 g) in ether (10 ml) and triethylamine (2 ml) were added to a stirred solution of N-benzoyl-N'-t-butyl hydrazine (1.0 g) in methylene chloride (3 ml). After stirring 5 minutes at room temperature, o-chloroaniline was added neat producing a mild exotherm. The reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml), separated and the organic washed with 0.1N HCl, dried over MgSO4, filtered and rotavapped to a colorless oil weighing 0.5 g.

후처리

  1. customproducing a mild exotherm
  2. customThe reaction was quenched 2 minutes later with water (20 ml) and ether (20 ml)
  3. customseparated
  4. washthe organic washed with 0.1N HCl
  5. dry with materialdried over MgSO4
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-622f237a76ee4662ac826ca1c7dcdf06
출처 데이터셋
uspto-grants-2000_01
특허 번호
US06013836

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