Hydrochloric Acid → Phosphine, bis(1,1-dimethylethyl)-

HRID 2287767

반응식

HRID 2287767 반응식
Cl[P:2]([C:7]([CH3:10])([CH3:9])[CH3:8])[C:3]([CH3:6])([CH3:5])[CH3:4].Cl.C1(C)C=CC=CC=1>CN(C)C=O.[Zn]>[C:3]([PH:2][C:7]([CH3:10])([CH3:9])[CH3:8])([CH3:6])([CH3:5])[CH3:4]

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 139566Di-tert-butylchlorophosphine

생성물 1

HCID 136643Phosphine, bis(1,1-dimethylethyl)-수율 25%

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 6228Dimethylformamide용매

실험 절차

0.849 g (4.70 mmol) of chloro-di-t-butylphosphine was added dropwise in a nitrogen gas atmosphere to a suspension of 461 mg (7.05 mg-atoms) of zinc (powder) in 10 cm3 of N,N-dimethylformamide and the mixture was stirred at room temperature for one hour. To the reaction mixture was added dropwise 10 cm3 (10 mmol) of 1 mol·dm-3 hydrochloric acid and then 10 cm3 of toluene. The mixture was stirred, the aqueous layer and the toluene layer were separated off, and the toluene layer was determined by gas chromatography, giving di-t-butylphosphine in 25% yield.

후처리

  1. stirringThe mixture was stirred
  2. customthe aqueous layer and the toluene layer were separated off

출처 및 근거

ORD 기록
ord-94fd5316d47f440a99ef8f7fc83fac1f
출처 데이터셋
uspto-grants-2000_07
특허 번호
US06084133

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