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Water → 1-(2-(Diphenylphosphanyl)phenyl)-N,N-dimethylmethanamine

HRID 329654
ノート
印刷プレビュー

反応式

HRID 329654 の反応式
[CH3:1][N:2]([CH3:10])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.C([Li])CCC.[Cl-].[C:17]1([PH:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.O>CCCCCC.CCOCC>[C:24]1([P:23]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[CH2:3][N:2]([CH3:10])[CH3:1])[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 7681N,N-DimethylbenzylamineHCID 19695023Diphenylphosphane chlorideHCID 178418339Butyllithium

生成物 1

HCID 113706101-(2-(Diphenylphosphanyl)phenyl)-N,N-dimethylmethanamine

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回
HCID 8058
Hexane
溶媒

実験手順

A 15.0 ml portion of N,N-dimethylbenzenemethanamine and 300 ml of ether were mixed under a nitrogen atmosphere. A 58 ml portion of 2.6M butyl lithium in hexane was added and this mixture was stirred, under nitrogen for 30 hours. A mixture of 27.0 ml of diphenylphosphine chloride in 60 ml of ether was added dropwise and the mixture was stirred overnight. Water was added, the organic layer was separated and extracted twice with dilute hydrochloric acid. The combined acid extracts were basified with 10% sodium hydroxide, then extracted twice with ether. The ether extracts were combined, dried and evaporated, giving 15.9 of 2-(diphenylphosphino)-N,N-dimethylbenzenemethanamine as an oil.

後処理

  1. additionwas added dropwise
  2. stirringthe mixture was stirred overnight
  3. customthe organic layer was separated
  4. extractionextracted twice with dilute hydrochloric acid
  5. extractionextracted twice with ether
  6. customdried
  7. customevaporated

出典と根拠

ORDレコード
ord-e2a9aa8ab8c842959e5338220bffece6
出典データセット
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04892885

反応ノート

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