反応 #74718

ord-636529bf8c044b80ad25cd39db528472

反応条件

温度
25°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度cooled to 5° C
  2. 2
    温度dropwise and with cooling
  3. 3
    workup.ADDITIONAfter the addition
  4. 4
    温度was heated to 95° C. for 2 hours
  5. 5
    workup.DISTILLATIONdistilling off a portion of the methanol
  6. 6
    温度The reaction was then cooled

実験手順

2-Acetyl-3-chloro-furan (1.0 g, 7 mmoles) in 30 ml methanol was cooled to 10° C. and 0.065 g, (1.7 mmoles) of NaBH4 added in one portion. After stirring for 30 minutes at 25° C., the solution was treated with 15 ml of water and cooled to 5° C. To the formed 2-(1-hydroxyethyl)-3-chloro-furan was then added 1.1 g (7 mmoles) of bromine, dropwise and with cooling. After the addition was complete the reaction was heated to 95° C. for 2 hours, distilling off a portion of the methanol. The reaction was then cooled and maltol isolated by the method of Example 1.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04173572uspto-grants-1979_11