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

HRID 1855963

反応式

HRID 1855963 の反応式
[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

参加物

6

反応物 4

HCID 1140Toluene2 回HCID 73122-(Diisopropylamino)ethyl chlorideHCID 24533Sodium amideHCID 14569341alpha-(4-Biphenylyl)-alpha-[2-(diisopropylamino)ethyl]acetonitrile

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-162dc3e4ad664e448fe0a75dfc4b50d9
出典データセット
uspto-grants-1980_08
特許番号
US04217306

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