Ammonium Hydroxide → HCID 86591986、化合物

HRID 1831534ノート

反応式

HRID 1831534 の反応式
[CH:1]1([CH:4]([NH:7][C:8]2[C:13]([N+:14]([O-])=O)=[C:12]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=3[CH3:25])[CH:11]=[CH:10][N:9]=2)[CH2:5][CH3:6])[CH2:3][CH2:2]1.[NH4+].[OH-].[O-]S(S([O-])=O)=O.[Na+].[Na+]>O1CCOCC1.O>[CH:1]1([CH:4]([NH:7][C:8]2[C:13]([NH2:14])=[C:12]([C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][C:18]=3[CH3:25])[CH:11]=[CH:10][N:9]=2)[CH2:5][CH3:6])[CH2:3][CH2:2]1

参加物

6

反応物 3

HCID 14923Ammonium HydroxideHCID 24489Sodium DithioniteHCID 22052063(1-Cyclopropyl-propyl)-[4-(4-methoxy-2-methyl-phenyl)-3-nitro-pyridin-2-yl]-amine

生成物 1

HCID 86591986HCID 86591986、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

(1-Cyclopropyl-propyl)-[4-(4-methoxy-2-methyl-phenyl)-3-nitro-pyridin-2-yl]-amine (0.220, 0.64 mmol) was dissolved in dioxane (10 mL) and H2O (10 mL), followed by conc. NH4OH (0.4 mL) and Na2S2O4 (0.906 g, 5.2 mmol) and stirred at room temperature for 4 h. The solution was extracted with EtOAc, washed with H2O, brine, dried Na2SO4, filtered, and concentrated in vacuo to produce the crude intermediate N2-(1-cyclopropyl-propyl)-4-(4-methoxy-2-methyl-phenyl)-pyridine-2,3-diamine; MS(AP) m/z 312.2 [(M+H)+, 100]. The crude intermediate was used in the following step.

後処理

  1. extractionThe solution was extracted with EtOAc
  2. washwashed with H2O, brine, dried Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8ee7a59acdd84483b697e471cc152b2c
出典データセット
uspto-grants-2006_06
特許番号
US07067658B2

反応ノート

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