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

HRID 2232406ノート

反応式

HRID 2232406 の反応式
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]

参加物

6

反応物 4

HCID 516892Sodium BicarbonateHCID 5998173-Chloro-4-nitropyridine N-oxideHCID 18759927N-[4-(piperazin-1-yl)phenyl]methanesulfonamide hydrochloride2 回HCID 21283535N-{4-[4-(4-Aminopyrid-2-yl)piperazin-1-yl]phenyl}methanesulphonamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

反応条件

温度
100 °C

実験手順

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%.

後処理

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

出典と根拠

ORDレコード
ord-83eaa1477f2840809921b8537ca37f28
出典データセット
uspto-grants-1988_11
特許番号
US04788196

反応ノート

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