2-Propanone, 1-nitro- → 4-(2-Benzylmercaptophenyl)-1,4-dihydro-2,6-dimethyl-5-nitropyridine-3-carboxylic acid N-[4-(6-oxo-1,4,5,6-tetrahydropyridazin-3-yl)-phenyl]-amide

HRID 247368ノート

反応式

HRID 247368 の反応式
[CH2:1]([S:8][C:9]1[CH:16]=[CH:15][CH:14]=[CH:13][C:10]=1[CH:11]=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[N+:17]([CH2:20][C:21](=O)[CH3:22])([O-:19])=[O:18].[O:24]=[C:25]1[NH:30][N:29]=[C:28]([C:31]2[CH:36]=[CH:35][C:34]([NH:37][C:38](=[O:43])/[CH:39]=[C:40](\[NH2:42])/[CH3:41])=[CH:33][CH:32]=2)[CH2:27][CH2:26]1>C(O)(C)C>[O:24]=[C:25]1[NH:30][N:29]=[C:28]([C:31]2[CH:32]=[CH:33][C:34]([NH:37][C:38]([C:39]3[CH:11]([C:10]4[CH:13]=[CH:14][CH:15]=[CH:16][C:9]=4[S:8][CH2:1][C:2]4[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=4)[C:20]([N+:17]([O-:19])=[O:18])=[C:21]([CH3:22])[NH:42][C:40]=3[CH3:41])=[O:43])=[CH:35][CH:36]=2)[CH2:27][CH2:26]1

参加物

5

反応物 3

HCID 662962-Propanone, 1-nitro-HCID 111178092-(Benzylsulfanyl)benzaldehydeHCID 70353925HCID 70353925、化合物

生成物 1

HCID 704356234-(2-Benzylmercaptophenyl)-1,4-dihydro-2,6-dimethyl-5-nitropyridine-3-carboxylic acid N-[4-(6-oxo-1,4,5,6-tetrahydropyridazin-3-yl)-phenyl]-amide

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

10 mmoles of 2-benzylmercaptobenzaldehyde, 15 mmoles of nitroacetone and 10 mmoles of 3-aminocrotonic acid N-[4-(6-oxo-1,4,5,6-tetrahydropyridazin-3-yl)-phenyl]-amide in 30 ml of isopropanol are heated at 60°-70° C. for 10 hours. The reaction mixture is concentrated and the residue is taken up in chloroform and chromatographed over silica gel using chloroform to which methanol is added. The product is recrystallized from isopropanol.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. customchromatographed over silica gel
  3. additionis added
  4. customThe product is recrystallized from isopropanol

出典と根拠

ORDレコード
ord-2f217b0ecf554432a8b63ae406eeb837
出典データセット
uspto-grants-1987_11
特許番号
US04707479

反応ノート

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