반응 #486227

ord-d867e2fdbf594cc1b9e3d464e6f84ac3

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The aqueous layer was separated
  2. 2
    추출extracted with diethyl ether (2×30 ml)
  3. 3
    세척The combined organic layers were washed with water
  4. 4
    건조dried over sodium sulfate
  5. 5
    농축concentrated in vacuo

실험 절차

To a solution of (±) cis-1-amino-2-[4-(1-methyl-1-phenylethyl)phenoxymethyl] cyclopentane (0.35 g, 1.13 mmol) in dry diethyl ether (30 ml) containing triethylamine (0.31 ml, 2.26 mmol) was added a solution of ethyl chloroformate (0.18 g, 1.70 mmol) in diethyl ether (5 ml). The reaction was stirred at room temperature for 2 h and then poured into ice-water. The pH of the aqueous phase was adjusted to approximately 7 by the addition of dilute hydrochloric acid. The aqueous layer was separated and extracted with diethyl ether (2×30 ml). The combined organic layers were washed with water followed by brine, then dried over sodium sulfate and concentrated in vacuo to give an oil (0.41 g) which was used in the next stage without purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05817698uspto-grants-1998_10