Acetic Acid → 4-(6-Chloronaphthalene-2-sulfonyl)-1-{ethyl[1-(4-pyridyl)-4-piperidinyl]amino}-2-piperazinone
반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:20][CH2:19][N:18]([NH:21][CH:22]3[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)[CH2:24][CH2:23]3)[C:17](=[O:34])[CH2:16]1)(=[O:14])=[O:13])[CH:6]=[CH:5]2.[BH4-].[Na+].[C:37](O)(=O)[CH3:38]>>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([S:12]([N:15]1[CH2:20][CH2:19][N:18]([N:21]([CH2:37][CH3:38])[CH:22]3[CH2:27][CH2:26][N:25]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)[CH2:24][CH2:23]3)[C:17](=[O:34])[CH2:16]1)(=[O:13])=[O:14])[CH:6]=[CH:5]2참가 물질
4
실험 절차
(Method B) 4-(6-Chloronaphthalene-2-sulfonyl)-1-[1-(4-pyridyl)-4-piperidinylamino]-2-piperazinone (14 g) was dissolved in acetic acid (160 ml) and the reaction mixture was treated portionwise with sodium borohydride (11.36 g) while keeping the temperature at 20° C., and then stirred at room temperature for 15 hours. The reaction mixture was concentrated and the residue was made alkaline by adding an aqueous solution of sodium hydroxide, extracted with dichloromethane, dried and concentrated. The residue obtained was crystallized from ethanol to obtain the title compound (12.96 g) as colorless crystals.
후처리
- customat 20° C.
- concentrationThe reaction mixture was concentrated
- additionby adding an aqueous solution of sodium hydroxide
- extractionextracted with dichloromethane
- customdried
- concentrationconcentrated
- customThe residue obtained
- customwas crystallized from ethanol
출처 및 근거
- ORD 기록
- ord-1c87c4d01b5a426abb3273c9e1d2896a
- 출처 데이터셋
- uspto-grants-2004_04
- 특허 번호
- US06723722B1
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