5-Amino-4-methyl-2-(1-methyl-piperidin-4-yl)-6-nitro-isoindole-1,3-dione → 5,6-Diamino-4-methyl-2-(1-methyl-piperidin-4-yl)-isoindole-1,3-dione

HRID 929090ノート

反応式

HRID 929090 の反応式
[NH2:1][C:2]1[C:3]([CH3:23])=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-])=O)[C:7](=[O:14])[N:6]([CH:15]1[CH2:20][CH2:19][N:18]([CH3:21])[CH2:17][CH2:16]1)[C:5]2=[O:22]>[Pd].CO>[NH2:1][C:2]1[C:3]([CH3:23])=[C:4]2[C:8](=[CH:9][C:10]=1[NH2:11])[C:7](=[O:14])[N:6]([CH:15]1[CH2:16][CH2:17][N:18]([CH3:21])[CH2:19][CH2:20]1)[C:5]2=[O:22]

参加物

4

反応物 1

HCID 597618595-Amino-4-methyl-2-(1-methyl-piperidin-4-yl)-6-nitro-isoindole-1,3-dione

生成物 1

HCID 597617275,6-Diamino-4-methyl-2-(1-methyl-piperidin-4-yl)-isoindole-1,3-dione収率 97.4%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

To a suspension of 5-Amino-4-methyl-2-(1-methyl-piperidin-4-yl)-6-nitro-isoindole-1,3-dione (1.7 g, 5.34 mmol) and 10% Pd/C (250 mg) was added MeOH (100 mL) carefully and evacuated in vacuo. The flask was filled with hydrogen under balloon pressure and stirred for 1 h. The reaction mixture was filtered and evaporated in vacuo to afford the crude 5,6-diamino-4-methyl-2-(1-methyl-piperidin-4-yl)-isoindole-1,3-dione (1.5 g, quant.), which was used as such for further reaction.

後処理

  1. customevacuated in vacuo
  2. additionThe flask was filled with hydrogen under balloon pressure
  3. filtrationThe reaction mixture was filtered
  4. customevaporated in vacuo

出典と根拠

ORDレコード
ord-6b510026dc694cabb4c27dec4b0adfc3
出典データセット
uspto-grants-2016_03
特許番号
US09290503B2

反応ノート

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