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

반응식

HRID 585483 반응식
[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]

참가 물질

6

반응물 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

생성물 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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-bdbb32fed643458fa56fb083084babee
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933296B2

연결된 노트

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