Potassium Carbonate → Aripiprazole

HRID 890336

반응식

HRID 890336 반응식
C(=O)([O-])[O-].[K+].[K+].Cl[CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]1[CH:22]=[C:21]2[C:16]([CH2:17][CH2:18][C:19](=[O:23])[NH:20]2)=[CH:15][CH:14]=1.Cl.[Cl:25][C:26]1[C:31]([Cl:32])=[CH:30][CH:29]=[CH:28][C:27]=1[N:33]1[CH2:38][CH2:37][NH:36][CH2:35][CH2:34]1>O>[CH:29]1[CH:28]=[C:27]([N:33]2[CH2:38][CH2:37][N:36]([CH2:8][CH2:9][CH2:10][CH2:11][O:12][C:13]3[CH:14]=[CH:15][C:16]4[CH2:17][CH2:18][C:19](=[O:23])[NH:20][C:21]=4[CH:22]=3)[CH2:35][CH2:34]2)[C:26]([Cl:25])=[C:31]([Cl:32])[CH:30]=1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 104674677-(4-Chlorobutoxy)-1,2,3,4-tetrahydroquinolin-2-oneHCID 116303721-(2,3-Dichlorophenyl)piperazine hydrochloride

생성물 1

HCID 60795Aripiprazole수율 92.8%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
92.5 °C

실험 절차

In 600 ml of water was dissolved 36.0 g of potassium carbonate, to which were added 60.0 g of 7-(4-chlorobutoxy)-3,4-dihydrocarbostyril and 69.6 g of 1-(2,3-dichlorophenyl)piperazine monohydrochloride. The mixture was heated with stirring at 90 to 95° C. for about 4 hours. Then, the reaction mixture was cooled to about 40° C., and the deposited crystals were collected by filtration. The crystals thus obtained were washed with 240 ml of water and dissolved in 900 ml of ethyl acetate, and an azeotropic mixture of water/ethyl acetate (about 300 ml) was distilled out under reflux. The remaining solution was cooled to 0 to 5° C., and the deposited crystals were collected by filtration. The crystals thus obtained were washed with 120 ml of ethyl acetate and dried under a reduced pressure of 50 Torr, at 50 to 60° C. for 3 hours to obtain 98.4 g of aripiprazole (yield 92.8%, purity 99%). mp. 140° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureThen, the reaction mixture was cooled to about 40° C.
  3. filtrationthe deposited crystals were collected by filtration
  4. customThe crystals thus obtained
  5. washwere washed with 240 ml of water
  6. dissolutiondissolved in 900 ml of ethyl acetate
  7. additionan azeotropic mixture of water/ethyl acetate (about 300 ml)
  8. distillationwas distilled out
  9. temperatureunder reflux
  10. temperatureThe remaining solution was cooled to 0 to 5° C.
  11. filtrationthe deposited crystals were collected by filtration
  12. customThe crystals thus obtained
  13. washwere washed with 120 ml of ethyl acetate
  14. customdried under a reduced pressure of 50 Torr, at 50 to 60° C. for 3 hours

출처 및 근거

ORD 기록
ord-e69d147e50854cc1a97fbcf42e5c0d6d
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995264B2

연결된 노트

불러오는 중…