Potassium Hydroxide → Risperidone

HRID 969738

반응식

HRID 969738 반응식
F[C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9](=[N:30][OH:31])[CH:10]1[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]2[C:23](=[O:24])[N:22]3[CH2:25][CH2:26][CH2:27][CH2:28][C:21]3=[N:20][C:19]=2[CH3:29])[CH2:12][CH2:11]1.[OH-].[K+]>O>[F:8][C:6]1[CH:5]=[CH:4][C:3]2[C:9]([CH:10]3[CH2:15][CH2:14][N:13]([CH2:16][CH2:17][C:18]4[C:23](=[O:24])[N:22]5[CH2:25][CH2:26][CH2:27][CH2:28][C:21]5=[N:20][C:19]=4[CH3:29])[CH2:12][CH2:11]3)=[N:30][O:31][C:2]=2[CH:7]=1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 71433889Risperidal iMpurity B

생성물 1

HCID 5073Risperidone수율 74.1%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 1 g (0.0023 mole) of 3-[2-[4-[(2,4-difluorophenyl)-(hydroxyimino)-methyl]-1-piperidinyl]ethyl]-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimidin-4-one and 1 g of potassium hydroxide in 10 ml of water is heated to boiling for an hour. The reaction mixture is cooled to room temperature and extracted twice with 10 ml of dichloromethane each. The organic phase is evaporated. Thus 0.70 g of 3-{2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl}-6,7,8,9-tetrahydro-2-methyl-4H-pyrido[1,2-a]pyrimid-in-4-one are obtained, yield 73.5%. According to HPLC analysis the purity of the product is 96.4%.

후처리

  1. waitto boiling for an hour
  2. extractionextracted twice with 10 ml of dichloromethane each
  3. customThe organic phase is evaporated

출처 및 근거

ORD 기록
ord-db9dd56ffd5543ad9519059b496683ad
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07307168B2

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