Hexane → alpha-(Cyclohexyl)-alpha,alpha-bis[2-(diisopropylamino)ethyl]acetamide

HRID 1855974ノート

反応式

HRID 1855974 の反応式
[CH:1]([N:4]([CH:26]([CH3:28])[CH3:27])[CH2:5][CH2:6][C:7]([CH2:17][CH2:18][N:19]([CH:23]([CH3:25])[CH3:24])[CH:20]([CH3:22])[CH3:21])([C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1)[C:8]([NH2:10])=[O:9])([CH3:3])[CH3:2].[H][H].CCCCCC>C(O)C.C(Cl)Cl.[Ru](=O)=O>[CH:11]1([C:7]([CH2:6][CH2:5][N:4]([CH:1]([CH3:3])[CH3:2])[CH:26]([CH3:28])[CH3:27])([CH2:17][CH2:18][N:19]([CH:20]([CH3:22])[CH3:21])[CH:23]([CH3:24])[CH3:25])[C:8]([NH2:10])=[O:9])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16]1

参加物

7

反応物 3

HCID 8058HexaneHCID 12612273alpha,alpha-Bis[2-(diisopropylamino)ethyl]-alpha-phenylacetamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 23347231alpha-(Cyclohexyl)-alpha,alpha-bis[2-(diisopropylamino)ethyl]acetamide

試薬・触媒・溶媒 3

HCID 82848Ruthenium dioxide触媒HCID 702Ethanol溶媒HCID 6344Dichloromethane溶媒2 回

反応条件

温度
125 °C

実験手順

10 Parts of α,α-bis[2-(diisopropylamino)ethyl]-α-phenylacetamide is dissolved in 130 parts by volume of ethanol and the solution placed in pressure shaker with 1 part of ruthenium dioxide. Hydrogen is introduced at 1000 psi and the reaction mixture heated at about 125° C. and shaken for about 24 hours. Then, the reaction mixture is cooled to room temperature and filtered. The filtrate is stripped of solvent to give an oil. This oil is dissolved in methylene chloride, then hexane added to the solution, methylene chloride evaporated, and the hexane mixture cooled to give α-(cyclohexyl)-α,α-bis[2-(diisopropylamino)ethyl]acetamide, as a crystal solid melting at about 114°-115° C. This compound has the following structural formula ##STR49##

後処理

  1. temperatureThen, the reaction mixture is cooled to room temperature
  2. filtrationfiltered
  3. customto give an oil
  4. customevaporated
  5. temperaturethe hexane mixture cooled

出典と根拠

ORDレコード
ord-123a16f7f1c3485f89dc95d12ea3e4ae
出典データセット
uspto-grants-1980_08
特許番号
US04217306

反応ノート

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