Ammonia → Donepezil Hydrochloride

HRID 456985

反応式

HRID 456985 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[CH2:9][CH:10]([CH2:13][CH:14]3[CH2:19][CH2:18][N:17]([CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=4)[CH2:16][CH2:15]3)[C:11](=[O:12])[C:6]2=[CH:5][C:4]=1[O:27][CH3:28].C(O)(C(O)=O)=O.[Cl:35]CCl.N>O>[CH3:1][O:2][C:3]1[CH:8]=[C:7]2[CH2:9][CH:10]([CH2:13][CH:14]3[CH2:15][CH2:16][N:17]([CH2:20][C:21]4[CH:22]=[CH:23][CH:24]=[CH:25][CH:26]=4)[CH2:18][CH2:19]3)[C:11](=[O:12])[C:6]2=[CH:5][C:4]=1[O:27][CH3:28].[ClH:35]

参加物

5

反応物 3

HCID 222AmmoniaHCID 6344DichloromethaneHCID 11397232Donepezil Oxalate

生成物 1

HCID 5741Donepezil Hydrochloride

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

Donepezil oxalate (purified, example 2), 5 gms, was dissolved in water 50 ml under heating at 50° C. Stirring was continued for 1 hour with gradual cooling. At room temperature, dichloromethane 50 ml was added and stirred for 10 mins. Liquid Ammonia 5 ml was added slowly with stirring. The dichloromethane layer was separated and 50 ml water was added to it. Analytical grade concentrated hydrochloric acid 1.5 ml was slowly added and stirred for 10 mins. Dichloromethane was distilled off under vacuum at 45° C. to obtain Donepezil hydrochloride in water, which was kept for lyophilyzation for 24 hours at −35° C. to give Donepezil hydrochloride amorphous with a yield of 3.9 gms (95%).

後処理

  1. stirringstirred for 10 mins
  2. stirringwith stirring
  3. customThe dichloromethane layer was separated
  4. addition50 ml water was added to it
  5. additionAnalytical grade concentrated hydrochloric acid 1.5 ml was slowly added
  6. stirringstirred for 10 mins
  7. distillationDichloromethane was distilled off under vacuum at 45° C.

出典と根拠

ORDレコード
ord-e33fa25e0ded41f99fecc6aa58b18729
出典データセット
uspto-grants-2007_03
特許番号
US07186842B2

関連ノート

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