Ethanol → 4-Methoxybenzoylacetonitrile

HRID 128167

反応式

HRID 128167 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([O:11][CH3:12])=[CH:7][CH:6]=1)=[O:4].C(O)C.[C-:16]#[N:17].[Na+]>O>[CH3:12][O:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]([CH2:2][C:16]#[N:17])=[O:4])=[CH:6][CH:7]=1

参加物

5

反応物 3

HCID 702EthanolHCID 4965Bromomethyl 4-methoxyphenyl ketoneHCID 8929Sodium Cyanide

生成物 1

HCID 2333984-Methoxybenzoylacetonitrile

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

A 25.0 g. portion of α-bromo-p-methoxyacetophenone is suspended in 125 ml. of ethanol. A solution of 16.0 g. of sodium cyanide in 75 ml. of water is added, using an ice-water bath to keep the temperature at 25°-30° C. The mixture is stirred for 45 minutes at room temperature. A total of 1.2 liters of water is added in 200 ml. increments with filtration through celite until no more precipitate forms. The filtrate is acidified to pH 5 with acetic acid. The solid is collected, washed with water, dried and recrystallized from benzene giving p-methoxybenzoylacetonitrile.

後処理

  1. customat 25°-30° C
  2. filtrationincrements with filtration through celite until no more precipitate forms
  3. customThe solid is collected
  4. washwashed with water
  5. customdried
  6. customrecrystallized from benzene

出典と根拠

ORDレコード
ord-16bcd28ed9d6423b87ecfbe629b634ca
出典データセット
uspto-grants-1981_03
特許番号
US04259256

関連ノート

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