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HRID69953

反应详情

EQUATION

反应方程式

HRID 69953 的结构方程式

REACTANTS

反应物

2
结构：CC1(C)OB(c2ccncc2N)OC1(C)C
HCID49760414

4-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-amine

C11H17BN2O2

结构：Cc1nc(Cl)cc(NC(=O)OC(C)(C)C)n1
HCID86669200

未命名化合物

PRODUCTS

生成物

1
结构：Cc1nc(NC(=O)OC(C)(C)C)cc(-c2ccncc2N)n1
HCID69047460

未命名化合物

收率 26%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：ClCCl.Cl[Pd]Cl.[Fe+2].c1ccc(P(c2ccccc2)[c-]2cccc2)cc1.c1ccc(P(c2ccccc2)[c-]2cccc2)cc1
催化剂HCID178418807

未命名化合物

结构：COCCOC
溶剂HCID8071

未命名化合物

PROCEDURE

实验过程

Method 26 was followed using tert-butyl 6-chloro-2-methylpyrimidin-4-ylcarbamate (1.0 equiv.), 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-3-amine (3.0 equiv.), Pd(dppf)Cl2-DCM (0.10 equiv.) in DME/2M Na2CO3 (3:1, 0.07M) at 80° C. for 30 min. Purification via SiO2 column chromatography eluting with EtOAc afforded tert-butyl 6-(3-aminopyridin-4-yl)-2-methylpyrimidin-4-ylcarbamate in 26% yield. LCMS (m/z): 302.1 (MH+); LC Rt=2.23 min.

WORKUP

后处理

  1. customat 80° C.
  2. customfor 30 min
  3. customPurification via SiO2 column chromatography
  4. washeluting with EtOAc