Sodium Bicarbonate → N-{4-[4-(4-Nitro-1-oxidopyrid-3-yl)piperazin-1-yl]phenyl}methanesulphonamide

HRID 2232406노트

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HRID 2232406 반응식
Cl.[N:2]1([C:8]2[CH:13]=[CH:12][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:10][CH:9]=2)[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.NC1C=CN=C(N2CCN(C3C=CC(NS(C)(=O)=O)=CC=3)CC2)C=1.Cl[C:44]1[CH:45]=[N+:46]([O-:53])[CH:47]=[CH:48][C:49]=1[N+:50]([O-:52])=[O:51].C(=O)(O)[O-].[Na+]>C(O)CCC>[N+:50]([C:49]1[CH:48]=[CH:47][N+:46]([O-:53])=[CH:45][C:44]=1[N:5]1[CH2:6][CH2:7][N:2]([C:8]2[CH:9]=[CH:10][C:11]([NH:14][S:15]([CH3:18])(=[O:17])=[O:16])=[CH:12][CH:13]=2)[CH2:3][CH2:4]1)([O-:52])=[O:51]

참가 물질

6

반응물 4

HCID 516892Sodium BicarbonateHCID 5998173-Chloro-4-nitropyridine N-oxideHCID 18759927N-[4-(piperazin-1-yl)phenyl]methanesulfonamide hydrochloride2회HCID 21283535N-{4-[4-(4-Aminopyrid-2-yl)piperazin-1-yl]phenyl}methanesulphonamide

생성물 1

HCID 21283522N-{4-[4-(4-Nitro-1-oxidopyrid-3-yl)piperazin-1-yl]phenyl}methanesulphonamide

시약·촉매·용매 1

HCID 2631-Butanol용매

반응 조건

온도
100 °C

실험 절차

A mixture of N-[(4-piperazin-1-yl)phenyl]methanesulphonamide hydrochloride (the product of Example 11, (iii) (0.59 g), 3-chloro-4-nitropyridine-N-oxide (0.35 g) and sodium bicarbonate (0.50 g) in n-butanol (25 ml) was heated at 100° C. with stirring for 1.5 hours and then evaporated. The residue was stirred with water, filtered, and the solid was crystallised from methanol to give the title compound (0.55 g), m.p. 206°-208° C. Found: C,48.77; H,4.91; N,17.52. C16H19N5O5S requires: C,48.84; H,4.87; N,17.80%.

후처리

  1. customevaporated
  2. stirringThe residue was stirred with water
  3. filtrationfiltered
  4. customthe solid was crystallised from methanol

출처 및 근거

ORD 기록
ord-83eaa1477f2840809921b8537ca37f28
출처 데이터셋
uspto-grants-1988_11
특허 번호
US04788196

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