HCID 14042135、化合物 → HCID 70097075、化合物

HRID 2368226ノート

反応式

HRID 2368226 の反応式
[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][CH:8]=[C:7]([C:12]2[CH:16]=[CH:15][O:14][CH:13]=2)[N:6]=1)=[O:4]>CO.[Pd]>[CH3:1][O:2][C:3]([C:5]1[C:10]([NH2:11])=[N:9][CH:8]=[C:7]([CH:12]2[CH2:16][CH2:15][O:14][CH2:13]2)[N:6]=1)=[O:4]

参加物

4

反応物 1

HCID 14042135HCID 14042135、化合物

生成物 1

HCID 70097075HCID 70097075、化合物

試薬・触媒・溶媒 2

HCID 23938Palladium触媒2 回HCID 887Methanol溶媒

実験手順

A solution of 3-amino-6-(furan-3-yl)-pyrazine-2-carboxylic acid methyl ester (2.9 g, 13.2 mmol) in MeOH (150 ml) was treated with palladium on carbon (10%; 0.6 g, 0.28 mmol) and hydrogenated at 1.2 atmospheres for 40 h. Another 2 equivalents of palladium on carbon were consecutively added and the hydrogenation was continued for another 72 h. The reaction mixture was filtered and the catalyst was washed with MeOH. The solution was concentrated in vacuo and the product was obtained after purification by silica gel chromatography using a heptane/ethyl acetate gradient as light yellow solid (0.3 g, 10%).

後処理

  1. waitthe hydrogenation was continued for another 72 h
  2. filtrationThe reaction mixture was filtered
  3. washthe catalyst was washed with MeOH
  4. concentrationThe solution was concentrated in vacuo
  5. customthe product was obtained
  6. customafter purification by silica gel chromatography

出典と根拠

ORDレコード
ord-41627f54c20b4d2caa09e104535e900b
出典データセット
uspto-grants-2014_04
特許番号
US08703768B2

反応ノート

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