Benzylamine → 4,6-dimethyl-7-hydroxy-1-benzylamino-2-phenyl-3H-indene

HRID 5000ノート

反応式

HRID 5000 の反応式
[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[C:7]2[C:3]=1[CH2:4][CH:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:6]2=O.[CH2:20]([NH2:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(OCC)C.ClCCl>[CH3:1][C:2]1[CH:10]=[C:9]([CH3:11])[C:8]([OH:12])=[C:7]2[C:3]=1[CH2:4][C:5]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)=[C:6]2[NH:27][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

参加物

5

反応物 2

HCID 7504BenzylamineHCID 140302654,6-Dimethyl-7-hydroxy-2-phenyl-1-indanone

生成物 1

HCID 150452594,6-dimethyl-7-hydroxy-1-benzylamino-2-phenyl-3H-indene

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

5.0 Grams of 4,6-dimethyl-7-hydroxy-2-phenyl-1-indanone was dissolved in 10 ml of diethyl ether and 10 ml of dichloromethane, then this solution was added dropwise gradually to a mixture of a solution of 2.55 ml of benzylamine in 10 ml of diethyl ether with 8 g of Molecular sieves 5A. The whole mixture was stirred at room temperature for 2 days and filtered by using Celite to obtain filtrate. The Celite used was washed with dichloromethane and ethanol, then these washing liquors were combined with the above-mentioned filtrate and concentrated. Recrystallized from dichloromethane-ethanol to obtain 3.83 g of 4,6-dimethyl-7-hydroxy-1-benzylamino-2-phenyl-3H-indene. Orange needle-like crystals.

後処理

  1. filtrationfiltered
  2. customto obtain filtrate
  3. washThe Celite used was washed with dichloromethane and ethanol
  4. concentrationconcentrated
  5. customRecrystallized from dichloromethane-ethanol

出典と根拠

ORDレコード
ord-502e59e83d8340a4bd3c79ffc19efc01
出典データセット
uspto-grants-1993_09
特許番号
US05242919

反応ノート

読み込み中…