Water → (4aS,8aR)-4-(3,4-Dimethoxy-phenyl)-2-[1-(2-ethenesulfonyl-ethyl)-piperidin-4-yl]-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one

HRID 585483

反応式

HRID 585483 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C@@H:20]3[C@@H:15]([CH2:16][CH:17]=[CH:18][CH2:19]3)[C:14](=[O:21])[N:13]([CH:22]3[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10].Br[CH2:29][CH2:30][S:31]([CH2:34][CH2:35]Br)(=[O:33])=[O:32].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([C:11]2[C@@H:20]3[C@@H:15]([CH2:16][CH:17]=[CH:18][CH2:19]3)[C:14](=[O:21])[N:13]([CH:22]3[CH2:27][CH2:26][N:25]([CH2:35][CH2:34][S:31]([CH:30]=[CH2:29])(=[O:33])=[O:32])[CH2:24][CH2:23]3)[N:12]=2)[CH:6]=[CH:7][C:8]=1[O:9][CH3:10]

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1390521-Bromo-2-(2-bromoethanesulfonyl)ethaneHCID 68878852(4aS,8aR)-4-(3,4-Dimethoxy-phenyl)-2-piperidin-4-yl-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one

生成物 1

HCID 69794500(4aS,8aR)-4-(3,4-Dimethoxy-phenyl)-2-[1-(2-ethenesulfonyl-ethyl)-piperidin-4-yl]-4a,5,8,8a-tetrahydro-2H-phthalazin-1-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 10 mmol of compound 5c, 10 mmol of 1-bromo-2-(2-bromo-ethanesulfonyl)-ethane and 30 mmol of potassium carbonate in 30 ml of dimethylformamide is stirred at RT. After 18 h, the mixture is poured into water (150 ml) and subsequently extracted with ethyl acetate. Crystallisation from diethyl ether. M. p. 165-166° C.

後処理

  1. extractionsubsequently extracted with ethyl acetate
  2. customCrystallisation from diethyl ether

出典と根拠

ORDレコード
ord-bdbb32fed643458fa56fb083084babee
出典データセット
uspto-grants-2005_08
特許番号
US06933296B2

関連ノート

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