Toluene → alpha-(4-Biphenylyl)-alpha,alpha-bis[2-(diisopropylamino)ethyl]acetonitrile

HRID 1855963노트

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HRID 1855963 반응식
[C:1]1([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[CH:6]=[CH:5][C:4]([CH:7]([CH2:10][CH2:11][N:12]([CH:16]([CH3:18])[CH3:17])[CH:13]([CH3:15])[CH3:14])[C:8]#[N:9])=[CH:3][CH:2]=1.C1(C)C=CC=CC=1.[NH2-].[Na+].Cl[CH2:35][CH2:36][N:37]([CH:41]([CH3:43])[CH3:42])[CH:38]([CH3:40])[CH3:39]>O>[C:1]1([C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=2)[CH:6]=[CH:5][C:4]([C:7]([CH2:35][CH2:36][N:37]([CH:41]([CH3:43])[CH3:42])[CH:38]([CH3:40])[CH3:39])([CH2:10][CH2:11][N:12]([CH:13]([CH3:14])[CH3:15])[CH:16]([CH3:18])[CH3:17])[C:8]#[N:9])=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 1140Toluene2회HCID 73122-(Diisopropylamino)ethyl chlorideHCID 24533Sodium amideHCID 14569341alpha-(4-Biphenylyl)-alpha-[2-(diisopropylamino)ethyl]acetonitrile

생성물 1

HCID 23347203alpha-(4-Biphenylyl)-alpha,alpha-bis[2-(diisopropylamino)ethyl]acetonitrile

시약·촉매·용매 1

HCID 962Water용매

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온도
100 °C

실험 절차

To a solution of 16 parts of α-(4-biphenylyl)-α-[2-(diisopropylamino)ethyl]acetonitrile in 150 parts by volume of toluene is added 2.7 parts of sodium amide and the solution is heated over a period of 15 minutes at about 100° C. Then 13 parts of 2-chloro-N,N-diisopropylethylamine in 40 parts by volume of toluene is added slowly over a period of 20 minutes. This mixture is heated at 100°-105° C. for about 90 minutes and then cooled to room temperature when 150 parts by volume of water is added. The organic layer is separated, dried over calcium sulfate, filtered and the solvent evaporated to afford α-(4-biphenylyl)-α,α-bis[2-(diisopropylamino)ethyl]acetonitrile, as a low melting solid. This compound is identical with the compound of Example 2, Method A.

후처리

  1. temperatureThis mixture is heated at 100°-105° C. for about 90 minutes
  2. additionis added
  3. customThe organic layer is separated
  4. dry with materialdried over calcium sulfate
  5. filtrationfiltered
  6. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-162dc3e4ad664e448fe0a75dfc4b50d9
출처 데이터셋
uspto-grants-1980_08
특허 번호
US04217306

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