반응 #2122541

ord-1a451d5ba21a4ef8a21fe375c3799789

반응 방정식

Cl
HCl
CC(C)(C)OC(=O)N1CCC[C@H]1c1ncc(-c2cnc(Cl)nc2)[nH]1
(S)-tert-butyl 2-(5-(2-chloropyrimidin-5-yl)-1H-imidazol-2-yl)pyrrolidine-1-carboxylate
Cl.Cl.Cl.Clc1ncc(-c2cnc([C@@H]3CCCN3)[nH]2)cn1
(S)-2-chloro-5-(2-(pyrrolidin-2-yl)-1H-imidazol-5-yl)pyrimidine trihydrochloride

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축was concentrated down to dryness
  2. 2
    workup.WAITplaced under high vacuum for 1 h

실험 절차

Cold (0° C.) 4 N HCl in dioxanes (5 mL) was added via syringe to (S)-tert-butyl 2-(5-(2-chloropyrimidin-5-yl)-1H-imidazol-2-yl)pyrrolidine-1-carboxylate (152d-1, 0.50 g, 1.43 mmol) in a 100 mL pear-shaped flask followed by MeOH (1.0 mL). The suspension was stirred at room temperature for 4 h before it was concentrated down to dryness and placed under high vacuum for 1 h. There was isolated intermediate (S)-2-chloro-5-(2-(pyrrolidin-2-yl)-1H-imidazol-5-yl)pyrimidine trihydrochloride as a pale yellow solid (with an orange tint) which was used without further purification.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08574563B2uspto-grants-2013_11