반응 #832352

ord-df8f6b140b294abab3af444106e85df7

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타the residue was partitioned between chloroform and water
  2. 2
    추출The chloroform layer was extracted with 10% sodium hydroxide
  3. 3
    기타After drying
  4. 4
    기타removal of solvent
  5. 5
    기타a brown oil was obtained which
  6. 6
    기타slowly crystallized
  7. 7
    기타recrystallized from methanol/diethyl ether

실험 절차

A solution of 2-diisopropylaminoethyl chloride hydrochloride (40.0 g, 0.2 mole) and potassium phthalimide (74.0 g, 0.4 mole) as stirred overnight at 85° C. in 500 ml of dimethyl formamide. The reaction mixture was stirred to dryness on a rotary evaporator, and the residue was partitioned between chloroform and water. The chloroform layer was extracted with 10% sodium hydroxide. After drying and removal of solvent, a brown oil was obtained which slowly crystallized. A portion of the oil was converted to the hydrochloride salt and recrystallized from methanol/diethyl ether to give 4.18 g (62.3%) of white crystalline product, m.p. 209°-211° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04597902uspto-grants-1986_07