반응 #53928

ord-22ce0e8d65a6428bb6e10a3a78ceabba

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타At 0° C.
  2. 2
    기타evaporated (2×)
  3. 3
    온도cooled (−10 to −15° C.)
  4. 4
    여과filtered

실험 절차

At 0° C., a solution of 4.4 g (12.63 mmol) of trans-[4-(5-Bromo-pentyl)-cyclohexyl]-carbamic acid tert-butyl ester were received in 9 m MeOH was added to 40 ml of a HBr solution in MeOH (made by dropping at 0° C., 4.7 ml (63.07 mmol) of acetylbromide to 35 ml MeOH). The suspension was stirred for 16 h at RT, diluted with toluene and evaporated (2×). The residue was suspended in EtOAc (40 ml) cooled (−10 to −15° C.) and filtered to give 4.05 g (97%) of trans-4-(5-Bromo-pentyl)-cyclohexylamine as hydrobromide salt, MS: 248 (MH+, 1Br).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06858651B2uspto-grants-2005_02