Diethyl Ether → 2-(2-Methoxy-5-cyanophenyl)-2-methyl-1-propanal

HRID 1155963

反応式

HRID 1155963 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6](Br)=[CH:5][C:4]=1[C:10]([CH3:14])([CH3:13])[CH:11]=[O:12].[CH3:15][N:16](C)C=O.C(OCC)C>O.Cl>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:15]#[N:16])=[CH:5][C:4]=1[C:10]([CH3:14])([CH3:13])[CH:11]=[O:12]

参加物

6

反応物 3

HCID 3283Diethyl EtherHCID 6228DimethylformamideHCID 205362232-(5-Bromo-2-methoxyphenyl)-2-methylpropanal

生成物 1

HCID 205362562-(2-Methoxy-5-cyanophenyl)-2-methyl-1-propanal

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

2-(2-Methoxy-5-bromophenyl)-2-methyl-1-propanal (9.5 g), prepared as in Example 5(d), cuprous cyanide (4.0 g) and dimethylformamide (20 ml) were heated under reflux with stirring for 3 hours. A solution of ferric chloride (7.3 g) in water (25 ml) and hydrochloric acid (3.5 ml conc) was added to the cooled reaction mixture which was then heated at 60°-70° C. for 5 minutes. Isolation of the product through diethyl ether yielded, after recrystallisation from ethanol, 3 g of pure product, mp 115°-117° C.

後処理

  1. temperaturewere heated
  2. temperatureunder reflux
  3. temperaturewas then heated at 60°-70° C. for 5 minutes
  4. customafter recrystallisation from ethanol, 3 g of pure product, mp 115°-117° C.

出典と根拠

ORDレコード
ord-07b1f9054299492899c6c5d2a13c790b
出典データセット
uspto-grants-1982_06
特許番号
US04333759

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