Triethylamine → O-(+)-menthyl dichlorophosphate

HRID 1741801

反応式

HRID 1741801 の反応式
[CH3:1][C@@H:2]1[CH2:7][C@H:6]([OH:8])[C@@H:5]([CH:9]([CH3:11])[CH3:10])[CH2:4][CH2:3]1.C(N(CC)CC)C.[O:19]=[P:20](Cl)([Cl:22])[Cl:21]>C1(C)C=CC=CC=1>[P:20]([Cl:22])([Cl:21])([O:8][CH:6]1[CH:5]([CH:9]([CH3:11])[CH3:10])[CH2:4][CH2:3][CH:2]([CH3:1])[CH2:7]1)=[O:19]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 24813Phosphorus oxychlorideHCID 165675(+)-Menthol

生成物 1

HCID 12473339O-(+)-menthyl dichlorophosphate収率 99%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A solution of 7.5 g (48 mmol) of (1S, 2R, 5S)-(+)-menthol (Aldrich) and 4.86 g (48 mmol) of triethylamine in 20 ml of toluene was dropped into 7.36 g (48 mmol) of POCl3 at 0° C. The entire solution was stirred for 23 hours at room temperature. The insoluble triethylamine hydrochloride was filtered and the solvent was evaporated. Yield 99%, 31P NMR δ 6.76 (CDCl3). (lit. T. Milobedzki, W. Janczak, Roczniki Chemji 11, 840 (1931)).

後処理

  1. filtrationThe insoluble triethylamine hydrochloride was filtered
  2. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-1fad478ae6fa49e19328d42f2e875834
出典データセット
uspto-grants-1994_08
特許番号
US05334741

関連ノート

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