Potassium Hydroxide → Risperidone

HRID 969738ノート

反応式

HRID 969738 の反応式
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

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 71433889Risperidal iMpurity B

生成物 1

HCID 5073Risperidone収率 74.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-db9dd56ffd5543ad9519059b496683ad
出典データセット
uspto-grants-2007_12
特許番号
US07307168B2

反応ノート

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