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

HRID 329654
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HRID 329654 반응식
[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
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참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회
HCID 8058
Hexane
용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e2a9aa8ab8c842959e5338220bffece6
출처 데이터셋
uspto-grants-1990_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04892885

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