Menthol → Dichloro((1R,2S,5R)-2-isopropyl-5-methylcyclohexyloxy)phosphine

HRID 41825

반응식

HRID 41825 반응식
[P:1]([Cl:4])(Cl)[Cl:2].[CH:5]1([CH3:15])[CH2:10][CH2:9][CH:8]([CH:11]([CH3:13])[CH3:12])[CH:7]([OH:14])[CH2:6]1>ClCCl>[Cl:2][P:1]([Cl:4])[O:14][C@@H:7]1[CH2:6][C@H:5]([CH3:15])[CH2:10][CH2:9][C@H:8]1[CH:11]([CH3:13])[CH3:12]

참가 물질

4

반응물 2

HCID 1254MentholHCID 24387Phosphorus trichloride

생성물 1

HCID 11054300Dichloro((1R,2S,5R)-2-isopropyl-5-methylcyclohexyloxy)phosphine수율 100%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
-30 °C

실험 절차

The phosphorus trichloride (56.0 ml, 87.89 g, 0.640 mol) was added to dichloromethane (anhydrous) under argon gas to obtain a solution. The solution was cooled to −30° C. and (−)-menthol (1R,2S,5R) (10.00 g, 0.0640 mol) was added portion wise over 10 mins. The solution was allowed to warm to ambient temperature and was allowed to stir at ambient temperature for 16 hours. The solvent was removed in vacuo to obtain a colourless oil (16.46 g). The crude product was used directly in the subsequent step.

후처리

  1. customto obtain a solution
  2. temperatureto warm to ambient temperature
  3. customThe solvent was removed in vacuo

출처 및 근거

ORD 기록
ord-418ec2ccf0174a49964151744e04de0f
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08535655B2

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