反应 #1256772

ord-d30fbe2da0e64b85a81f62b3bb31ba9f

反应方程式

CC(C)(C)OC(=O)N[C@H]1CC[C@H](CCN2CCN(c3noc4ccncc34)CC2)CC1
{trans-4-[2-(4-Isoxazolo[4,5-c]pyridin-3-yl-piperazin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester
Cl
HCl
C1COCCO1
dioxane
Cl.Cl.N[C@H]1CC[C@H](CCN2CCN(c3noc4ccncc34)CC2)CC1
trans-4-[2-(4-Isoxazolo[4,5-c]pyridin-3-yl-piperazin-1-yl)-ethyl]-cyclohexylamine dihydrochloride

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    过滤After dilution with iPr2O the product was collected by filtration
  2. 2
    洗涤washed with one portion of iPr2O
  3. 3
    其他before drying it under high vacuum at 50° C.
  4. 4
    其他to obtain 686 mg (79%) as a white solid

实验过程

{trans-4-[2-(4-Isoxazolo[4,5-c]pyridin-3-yl-piperazin-1-yl)-ethyl]-cyclohexyl}-carbamic acid tert-butyl ester (930 mg, 2.2 mmol) was dissolved in CH2Cl2 (3 ml) and 4 N HCl in dioxane (10.8 ml, 43 mmol) was added. The resulting mixture was stirred 16 h at r.t. After dilution with iPr2O the product was collected by filtration and washed with one portion of iPr2O before drying it under high vacuum at 50° C. to obtain 686 mg (79%) as a white solid. m/z=330.3 ([M+H]+).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07825123B2uspto-grants-2010_11