تفاعل #53928

ord-22ce0e8d65a6428bb6e10a3a78ceabba

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    أخرىAt 0° C.
  2. 2
    أخرىevaporated (2×)
  3. 3
    درجة الحرارةcooled (−10 to −15° C.)
  4. 4
    ترشيحfiltered

الإجراء التجريبي

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).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US06858651B2uspto-grants-2005_02