Ammonium formate → 6-(4-Methylpiperazin-1-yl)-4-(propan-2-yloxy)pyridin-3-amine

HRID 518830ノート

反応式

HRID 518830 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:13]=[C:12]([O:14][CH:15]([CH3:17])[CH3:16])[C:11]([N+:18]([O-])=O)=[CH:10][N:9]=2)[CH2:4][CH2:3]1.C([O-])=O.[NH4+]>[Pd].CO>[CH3:1][N:2]1[CH2:7][CH2:6][N:5]([C:8]2[N:9]=[CH:10][C:11]([NH2:18])=[C:12]([O:14][CH:15]([CH3:17])[CH3:16])[CH:13]=2)[CH2:4][CH2:3]1

参加物

5

反応物 2

HCID 2723923Ammonium formateHCID 866979951-Methyl-4-[5-nitro-4-(propan-2-yloxy)pyridin-2-yl]piperazine

生成物 1

HCID 866979966-(4-Methylpiperazin-1-yl)-4-(propan-2-yloxy)pyridin-3-amine収率 97.6%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

反応条件

温度
80 °C

実験手順

In a microwave tube, 390 mg of 1-methyl-4-[5-nitro-4-(propan-2-yloxy)pyridin-2-yl]piperazine are introduced into 12 ml of methanol. 525 mg of ammonium formate and 210 mg of Pd/C (10%) are added. The reaction medium is microwave-heated at 80° C. for 5 minutes. The mixture is filtered on Clarcel and the Clarcel is rinsed with methanol. The filtrate is concentrated under reduced pressure, so as to give 340 mg of 6-(4-methylpiperazin-1-yl)-4-(propan-2-yloxy)pyridin-3-amine in the form of a brown oil.

後処理

  1. filtrationThe mixture is filtered on Clarcel
  2. washthe Clarcel is rinsed with methanol
  3. concentrationThe filtrate is concentrated under reduced pressure

出典と根拠

ORDレコード
ord-f99c49cdc04b4d4fbcc42958b91200db
出典データセット
uspto-grants-2015_08
特許番号
US09115140B2

反応ノート

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