반응 #72528

ord-ac96ec0ecba344c39e16f6c953d0cc35

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The solution is cooled to 0° C.
  2. 2
    추출After extraction with DCM
  3. 3
    세척the organic phases are washed with water and with saturated aqueous NaCl solution
  4. 4
    건조dried over sodium sulphate
  5. 5
    여과filtered
  6. 6
    기타evaporated to dryness

실험 절차

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.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541412B2uspto-grants-2013_09