反応 #72528

ord-ac96ec0ecba344c39e16f6c953d0cc35

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The solution is cooled to 0° C.
  2. 2
    抽出After extraction with DCM
  3. 3
    洗浄the organic phases are washed with water and with saturated aqueous NaCl solution
  4. 4
    乾燥dried over sodium sulphate
  5. 5
    ろ過filtered
  6. 6
    その他evaporated to dryness

実験手順

To a solution of morpholine (22 mmoles) in acetic acid (10 ml) there is added pyrrole (20 mmoles) dropwise at 0° C. Formaldehyde (37% aq., 20 mmoles) is then added dropwise. The reaction mixture is stirred for 2 hours at ambient temperature. The solution is cooled to 0° C. and is brought to alkaline pH (10-11) using 20% aqueous NaOH solution. After extraction with DCM, the organic phases are washed with water and with saturated aqueous NaCl solution, dried over sodium sulphate, filtered and evaporated to dryness to yield the title product in the form of a white solid which is used directly in the next Step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08541412B2uspto-grants-2013_09