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

HRID 41825

反応式

HRID 41825 の反応式
[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]

参加物

4

反応物 2

HCID 1254MentholHCID 24387Phosphorus trichloride

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
-30 °C

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-418ec2ccf0174a49964151744e04de0f
出典データセット
uspto-grants-2013_09
特許番号
US08535655B2

関連ノート

読み込み中…