Ammonia → Donepezil Hydrochloride

HRID 456985

반응식

HRID 456985 반응식
[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]

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 6344DichloromethaneHCID 11397232Donepezil Oxalate

생성물 1

HCID 5741Donepezil Hydrochloride

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
50 °C

실험 절차

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%).

후처리

  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.

출처 및 근거

ORD 기록
ord-e33fa25e0ded41f99fecc6aa58b18729
출처 데이터셋
uspto-grants-2007_03
특허 번호
US07186842B2

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