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Sodium borohydride → Paliperidone

HRID 448542
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HRID 448542 반응식
[F:1][C:2]1[CH:31]=[CH:30][C:5]2[C:6]([CH:9]3[CH2:14][CH2:13][N:12]([CH2:15][CH2:16][C:17]4[C:22](=[O:23])[N:21]5[CH2:24][CH2:25][CH2:26][C:27](=[O:28])[C:20]5=[N:19][C:18]=4[CH3:29])[CH2:11][CH2:10]3)=[N:7][O:8][C:4]=2[CH:3]=1.[BH4-].[Na+]>CO.ClCCl>[CH3:29][C:18]1[N:19]=[C:20]2[N:21]([CH2:24][CH2:25][CH2:26][CH:27]2[OH:28])[C:22](=[O:23])[C:17]=1[CH2:16][CH2:15][N:12]1[CH2:13][CH2:14][CH:9]([C:6]2[C:5]3[CH:30]=[CH:31][C:2]([F:1])=[CH:3][C:4]=3[O:8][N:7]=2)[CH2:10][CH2:11]1
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5

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HCID 4311764Sodium borohydrideHCID 446083593-{2-[4-(6-Fluoro-1,2-benzoxazol-3-yl)piperidin-1-yl]ethyl}-2-methyl-7,8-dihydro-4H-pyrido[1,2-a]pyrimidine-4,9(6H)-dione

생성물 1

HCID 115237Paliperidone

시약·촉매·용매 2

HCID 887Methanol용매HCID 6344Dichloromethane용매

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온도
30 °C

실험 절차

To a solution of 3-[2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidin-1-yl]ethyl]-9-oxo-2-methyl-6,7,8,9-tetrahydro-4H-pyrido-[1,2-a]pyrimidin-4-one (formula-10) (0.3 grams) taken in a mixture of methanol (1.5 ml) and dichloromethane (3 ml) added sodium borohydride (0.008 grams) and stirred for 1 hour at 30° C. The solvent was distilled off under reduced pressure. Methanol (1.5 ml) was added to it and heated to reflux for 30 min. the reaction mixture was cooled to 20° C. and stirred for 1 hour. Filtered the solid, washed with methanol and dried.

후처리

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionMethanol (1.5 ml) was added to it
  3. temperatureheated
  4. temperatureto reflux for 30 min. the reaction mixture
  5. temperaturewas cooled to 20° C.
  6. stirringstirred for 1 hour
  7. filtrationFiltered the solid
  8. washwashed with methanol
  9. customdried

출처 및 근거

ORD 기록
ord-31fcfda66c1e45ac94a75421d21bf066
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481729B2

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