Propanal → p-Azido-2-methylcinnamaldehyde

HRID 1885047

反応式

HRID 1885047 の反応式
[N:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=O)=[CH:6][CH:5]=1)=[N+:2]=[N-:3].[CH:12](=[O:15])[CH2:13]C.[OH-].[Na+].[CH:18](O)(C)C>O>[N:1]([C:4]1[CH:11]=[CH:10][C:7]([CH:8]=[CH:13][CH:12]=[O:15])=[C:6]([CH3:18])[CH:5]=1)=[N+:2]=[N-:3]

参加物

6

反応物 4

HCID 527Propanal2 回HCID 3776IsopropanolHCID 14798Sodium HydroxideHCID 903854-Azidobenzaldehyde

生成物 1

HCID 86589921p-Azido-2-methylcinnamaldehyde収率 62%

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

4-Azidobenzaldehyde (29.42 g, 0.2 mol) and propionaldehyde (12.22 g, 0.2 mol) were dissolved in a solvent mixture of isopropyl alcohol (100 g) and pure water (50 g). Under cooling in an ice bath, sodium hydroxide (2 g) dissolved in pure water (20 g) was added to the solution, and the mixture was stirred for two hours. Propionaldehyde (12.22 g, 0.2 mol) was added again to the mixture, and the resultant mixture was stirred for a further three hours. The formed precipitates were collected through filtration and dried, to thereby yield 23.14 g of p-azido-2-methylcinnamaldehyde as yellow crystals (yield: 62%). The compound thus obtained was identified on the basis of the 1H-NMR measurements shown in Table 1.

後処理

  1. temperatureUnder cooling in an ice bath
  2. additionwas added to the solution
  3. customThe formed precipitates
  4. filtrationwere collected through filtration
  5. customdried

出典と根拠

ORDレコード
ord-cba7d836589841a992d0f75199a96b65
出典データセット
uspto-grants-2004_07
特許番号
US06768027B2

関連ノート

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