Propylamine → (1-Phenylpentan-2-yl)(propyl)amine

HRID 1461412ノート

反応式

HRID 1461412 の反応式
[CH2:1]([C:8]([CH2:10][CH2:11][CH3:12])=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:13]([NH2:16])[CH2:14][CH3:15].[Cl-].[Ca+2].[Cl-].[BH4-].[Na+]>C1C=CC=CC=1.CO.O>[CH2:13]([NH:16][CH:8]([CH2:10][CH2:11][CH3:12])[CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[CH2:14][CH3:15]

参加物

8

反応物 4

HCID 7852PropylamineHCID 811881-Phenyl-2-pentanoneHCID 4311764Sodium borohydrideHCID 5284359Calcium Chloride

生成物 1

HCID 10262369(1-Phenylpentan-2-yl)(propyl)amine

試薬・触媒・溶媒 3

HCID 241Benzene溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

11.0 g (0.068 mole) of benzyl-propyl-ketone are dissolved in 110 ml of benzene, whereupon 8.0 g (0.135 mole) of n-propylamine and 22.6 g (0.2 mole) of anhydrous calcium chloride are added to the solution. The reaction mixture is stirred at 40°-50° C. for 6 hours, then filtered and evaporated. The crude ketimine thus obtained is dissolved in 120 ml of methanol, whereupon 6.4 g (0.17 mole) of sodium borohydride are added. The reaction mixture is allowed to stand, whereupon it is poured into 500 ml of water and extracted five times with 100 of benzene each. The benzene solution is dried and evaporated. The crude N-propyl-1-phenyl-2-pentylamine thus obtained is purified by distillation in vacuo. B.p.: 112°-120° C./7 Hgmm, n20D =1.5030.

後処理

  1. additionare added to the solution
  2. filtrationfiltered
  3. customevaporated
  4. customThe crude ketimine thus obtained
  5. additionare added
  6. extractionextracted five times with 100 of benzene each
  7. dry with materialThe benzene solution is dried
  8. customevaporated

出典と根拠

ORDレコード
ord-19da264f11cd4ad28a71986b271d143c
出典データセット
uspto-grants-1991_12
特許番号
US05075338

反応ノート

読み込み中…