تفاعل #72528

ord-ac96ec0ecba344c39e16f6c953d0cc35

معادلة التفاعل

C1COCCN1
morpholine
c1cc[nH]c1
pyrrole
[Na+].[OH-]
NaOH
C=O
Formaldehyde
c1c[nH]c(CN2CCOCC2)c1
title product
c1c[nH]c(CN2CCOCC2)c1
4-(1H-Pyrrol-2-ylmethyl)-morpholine

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةThe solution is cooled to 0° C.
  2. 2
    استخلاصAfter extraction with DCM
  3. 3
    غسيلthe organic phases are washed with water and with saturated aqueous NaCl solution
  4. 4
    تجفيفdried over sodium sulphate
  5. 5
    ترشيحfiltered
  6. 6
    أخرىevaporated to dryness

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08541412B2uspto-grants-2013_09