Formate → 3-Hydroxy-3-methylglutaric acid monoamide

HRID 1706591ノート

反応式

HRID 1706591 の反応式
[OH:1][C:2]([CH3:9])([CH2:6]C#N)[CH2:3][C:4]#[N:5].[OH:10]O.[CH:12]([O-:14])=[O:13]>[OH-].[Na+].O>[OH:1][C:2]([CH3:9])([CH2:6][C:12]([OH:14])=[O:13])[CH2:3][C:4]([NH2:5])=[O:10]

参加物

6

反応物 3

HCID 283FormateHCID 784Hydrogen PeroxideHCID 127207073-Hydroxy-3-methylpentanedinitrile

生成物 1

HCID 127207103-Hydroxy-3-methylglutaric acid monoamide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 14798Sodium Hydroxide溶媒

実験手順

A solution of 12.4 g (0.10 moles) of 3-hydroxy-3-methylglutaronitrile in 107 ml of 1.3 M sodium hydroxide is stirred at room temperature while 17.4 ml (0.20 moles) of 30% hydrogen peroxide is slowly added. After the addition of peroxide, the mixture is heated to boiling and boiling is maintained for 2 hours. Thereafter the mixture is cooled, diluted to 1 liter with water and passed through a 200 ml column of Dowex 2 resin in the formate form. The column is then washed with 1 liter of water. Thereafter the product is eluted with 1 liter of 0.1 N formic acid and the eluate evaporated to dryness to afford 3-hydroxy-3-methylglutaric acid monoamide.

後処理

  1. additionis slowly added
  2. temperaturethe mixture is heated
  3. temperatureboiling is maintained for 2 hours
  4. temperatureThereafter the mixture is cooled
  5. washThe column is then washed with 1 liter of water
  6. washThereafter the product is eluted with 1 liter of 0.1 N formic acid
  7. customthe eluate evaporated to dryness

出典と根拠

ORDレコード
ord-a59c5a65fb1443c28d52f3c1dcc61690
出典データセット
uspto-grants-1980_06
特許番号
US04208204

反応ノート

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