反応 #1057433

ord-b13c7fc6917c4f9c82d42f288b054d13

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The precipitate was collected on
  2. 2
    ろ過a filter
  3. 3
    洗浄washed with 50 ml of ethanol
  4. 4
    workup.ADDITIONThen the solid was mixed with 1.5 ml of concentrated hydrochloric acid and 35 ml of ethanol
  5. 5
    workup.STIRRINGIt was stirred for 30 min
  6. 6
    その他the product was collected on a filter
  7. 7
    洗浄After washing with 50 ml of ethanol
  8. 8
    乾燥drying in a dessicator 4.1 g of the product
  9. 9
    その他were obtained (yield 38%)

実験手順

0.43 g (62 mmole) of Li was dissolved in 180 ml of ethanol under a nitrogen atmosphere. Then 6.9 g (31 mmole) of 4-(6-hydroxyhexyloxy)-benzaldehyde (15) and 14.8 g (31 mmole) of (4-carboxy-benzyl)-triphenylphosphonium bromide (14) were added. The mixture was stirred for two hours at room temperature. The precipitate was collected on a filter and washed with 50 ml of ethanol. Then the solid was mixed with 1.5 ml of concentrated hydrochloric acid and 35 ml of ethanol. It was stirred for 30 min and the product was collected on a filter. After washing with 50 ml of ethanol and drying in a dessicator 4.1 g of the product were obtained (yield 38%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07311948B2uspto-grants-2007_12