Ethanol → HCID 67608342、化合物

HRID 925289ノート

反応式

HRID 925289 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([C:9]#[N:10])[N:6]=[C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH:4]=1.C([O-])=O.[NH4+].C(O)C>O.[OH-].[Pd+2].[OH-].[Pd]>[CH3:1][O:2][C:3]1[CH:8]=[C:7]([CH2:9][NH2:10])[N:6]=[C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)[CH:4]=1

参加物

6

反応物 3

HCID 702EthanolHCID 2723923Ammonium formateHCID 135867984-Methoxy[2,2′-bipyridine]-6-carbonitrile

生成物 1

HCID 67608342HCID 67608342、化合物

試薬・触媒・溶媒 2

HCID 86707187HCID 86707187、化合物触媒HCID 962Water溶媒

反応条件

温度
27 °C

実験手順

A mixture of 4-Methoxy-[2,2′]bipyridinyl-6-carbonitrile (1.0 g, 4.73 mmol), Palladium hydroxide-Pd 20%-50% in water (0.66 g, excess), ammonium formate (1.5 g, excess) and ethanol (60 mL) was stirred at 27° C. for 2 hours. The reaction was then filtered thorough celite, washed with methanol (150 mL) and dichloromethane (150 mL) and the organic phase evaporated to dryness affording C-(4-Methoxy-[2,2′]bipyridinyl-6-yl)-methylamine as an orange oil (0.80 g, 45%, in a ratio 72 to 28 product vs. byproduct).

後処理

  1. filtrationThe reaction was then filtered thorough celite
  2. washwashed with methanol (150 mL) and dichloromethane (150 mL)
  3. customthe organic phase evaporated to dryness

出典と根拠

ORDレコード
ord-10b15ff6da5b48f09413dff1e52b33f7
出典データセット
uspto-grants-2016_03
特許番号
US09284296B2

反応ノート

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