Tetrahydrofuran → Risperidone

HRID 969737

반응식

HRID 969737 반응식
[H-].[Na+].O1CCCC1.F[C:9]1[CH:14]=[C:13]([F:15])[CH:12]=[CH:11][C:10]=1[C:16](=[N:37][OH:38])[CH:17]1[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][C:25]2[C:30](=[O:31])[N:29]3[CH2:32][CH2:33][CH2:34][CH2:35][C:28]3=[N:27][C:26]=2[CH3:36])[CH2:19][CH2:18]1>O>[F:15][C:13]1[CH:12]=[CH:11][C:10]2[C:16]([CH:17]3[CH2:22][CH2:21][N:20]([CH2:23][CH2:24][C:25]4[C:30](=[O:31])[N:29]5[CH2:32][CH2:33][CH2:34][CH2:35][C:28]5=[N:27][C:26]=4[CH3:36])[CH2:19][CH2:18]3)=[N:37][O:38][C:9]=2[CH:14]=1

참가 물질

5

반응물 3

HCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 71433889Risperidal iMpurity B

생성물 1

HCID 5073Risperidone수율 77%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a suspension of 40 mg (0.9166 millimole) of 55% sodium hydride and 2 ml of tetrahydrofurane 0.1089 g (0.2532 millimole) 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 is added. The reaction mixture is heated to boiling for an hour, whereupon 5 ml of water are added and the mixture is extracted twice with 10 ml of dichloromethane each. The combined organic phases are dried over magnesium sulfate and evaporated in vacuo. Thus 80 mg of the title compound are obtained, yield 77%. According to HPLC analysis the purity of the product is 97.5%.

후처리

  1. additionis added
  2. temperatureThe reaction mixture is heated
  3. additionare added
  4. extractionthe mixture is extracted twice with 10 ml of dichloromethane each
  5. dry with materialThe combined organic phases are dried over magnesium sulfate
  6. customevaporated in vacuo

출처 및 근거

ORD 기록
ord-08ce3ee00e0c4bee98be53ed511da509
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07307168B2

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