反応 #69602

ord-803a1df4ba5f4e028f869e71911b3ae9

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The organic layer was separated
  2. 2
    抽出the aqueous layer was extracted with 2×150 mL of water
  3. 3
    洗浄The combined organic extracts were washed with aqueous NaHCO3
  4. 4
    乾燥dried over Na2SO4
  5. 5
    その他evaporated to dryness

実験手順

To a solution of 32.3 g (138 mmol) of 7 in 150 mL of dry diethyl ether, 24.8 g (8.62 mL, 91.6 mmol) of PBr3 was added at −10° C. The resulting mixture was stirred for 12 hr at room temperature and then added to 450 mL of cold water. The organic layer was separated, and the aqueous layer was extracted with 2×150 mL of water. The combined organic extracts were washed with aqueous NaHCO3, dried over Na2SO4, and then evaporated to dryness. This procedure gave 37.7 g (92%) of 8.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530593B2uspto-grants-2013_09