Formaldehyde → 5-{[N-methyl-N-(2-propynyl)amino]methyl}-2-furanmethanol

HRID 2418028ノート

反応式

HRID 2418028 の反応式
[CH2:1]([OH:7])[C:2]1[O:6][CH:5]=[CH:4][CH:3]=1.Cl.[CH3:9][NH:10][CH2:11][C:12]#[CH:13].[CH2:14]=O.[OH-].[Na+]>>[CH3:9][N:10]([CH2:14][C:5]1[O:6][C:2]([CH2:1][OH:7])=[CH:3][CH:4]=1)[CH2:11][C:12]#[CH:13]

参加物

5

反応物 4

HCID 712FormaldehydeHCID 7361Furfuryl AlcoholHCID 14798Sodium HydroxideHCID 22416630HCID 22416630、化合物

生成物 1

HCID 131029015-{[N-methyl-N-(2-propynyl)amino]methyl}-2-furanmethanol

実験手順

To furfuryl alcohol (2.49 g; 25.4 mmoles) which was cooled in an ice-water bath to 5° was added N-methylpropargylamine hydrochloride (4.0 g; 37.9 mmoles) and 40% formalin (3.13 ml; 41.7 mmoles), and the mixture stirred while allowed to reach ambient temperature. After 1 hour of stirring the solution was allowed to stand at ambient temperature for 41/2 days. The reaction mixture was poured into ice water, made strongly basic with 40% aqueous NaOH and extracted with five portions of methylene chloride. The combined organic phase was dried, filtered and evaporated under reduced pressure to give the product as an oil (quantitative yield). Vacuum distillation yielded the title compound, bp 102°-106°/0.3 mm Hg.

後処理

  1. customto reach ambient temperature
  2. stirringAfter 1 hour of stirring the solution
  3. customto stand at ambient temperature for 41
  4. custom2 days
  5. extractionextracted with five portions of methylene chloride
  6. customThe combined organic phase was dried
  7. filtrationfiltered
  8. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-929adb11e8984c8b83d9b1815673e94a
出典データセット
uspto-grants-1984_09
特許番号
US04471122

反応ノート

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