Ammonia → 1-(2-Methyl-5-pyridyl)-3-amino-but-2-en-1-one

HRID 918065

反応式

HRID 918065 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]([OH:13])[CH2:9][CH:10]([NH2:12])[CH3:11])=[CH:4][N:3]=1.CC1C=CC(C(CC(=O)C)=O)=CN=1.[Br-].[NH4+].N.B([O-])=O.[Na+]>C(O)C>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH:9]=[C:10]([NH2:12])[CH3:11])=[CH:4][N:3]=1

参加物

7

反応物 5

HCID 222Ammonia2 回HCID 25514Ammonium BromideHCID 145326Sodium metaborateHCID 202128141-(6-Methylpyridin-3-yl)butane-1,3-dioneHCID 544307431-(2-Methyl-5-pyridyl)-3-amino-n-butanol

生成物 1

HCID 681359721-(2-Methyl-5-pyridyl)-3-amino-but-2-en-1-one

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

1-(2-Methyl-5-pyridyl)-3-amino-n-butanol can be used as the starting material, is obtained as follows: 20.0 g of (6-methyl-nicotinoyl)-acetone, 200 ml of ethanol and 0.5 g of ammonium bromide are saturated with ammonia at 50° and heated at 50° for 15 hours whilst continuing to introduce ammonia. 8.5 g of sodium boranate are introduced in portions over the course of 1 hour into the solution, obtained above, of 1-(2-methyl-5-pyridyl)-3-amino-but-2-en-1-one of the formula ##EQU46## and the mixture is stirred for 7 hours at 70° . The solvent is distilled off in vacuo and the residue is taken up in 20% strength aqueous potassium hydroxide solution and pentanol-1. After working up in the usual manner, 19.2 g of crude 1-(2-methyl-5-pyridyl)-3-amino-n-butanol of the formula ##EQU47## are obtained from the pentanol solution as an oil which can be purified further by column chromatography.

後処理

  1. customis obtained
  2. temperatureheated at 50° for 15 hours

出典と根拠

ORDレコード
ord-33b53f02418b48518ef71bac0104e40a
出典データセット
uspto-grants-1976_07
特許番号
US03969363

関連ノート

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