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HRID1894331

反应详情

EQUATION

反应方程式

HRID 1894331 的结构方程式

REACTANTS

反应物

1
结构：CCOc1nc(C(C)(C)C)ncc1C1=N[C@@](C)(c2ccc(Cl)cc2)[C@@](C)(c2ccc(Cl)cc2)N1C(=O)N1CCN(CC[C@@H]2COC(C)(C)O2)CC1
HCID68942827

未命名化合物

PRODUCTS

生成物

1
结构：CCOc1nc(C(C)(C)C)ncc1C1=NC(C)(c2ccc(Cl)cc2)C(C)(c2ccc(Cl)cc2)N1C(=O)N1CCN(CC[C@@H](O)CO)CC1
HCID25262283

未命名化合物

收率 23.3%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：O=C(O)C(F)(F)F
催化剂HCID6422

未命名化合物

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

To a solution of rac-[(4S*,5R*)-2-(2-tert-butyl-4-ethoxy-pyrimidin-5-yl)-4,5-bis-(4-chloro-phenyl)-4,5-dimethyl-4,5-dihydro-imidazol-1-yl]-{4-[2-((R)-2,2-dimethyl-[1,3]dioxolan-4-yl)-ethyl]-piperazin-1-yl}-methanone (30 mg) in tetrahydrofuran (1 mL) was added 10 drops of trifluoroacetic acid. The mixture was stirred at room temperature for 2 d and concentrated. Purification of the crude residue by reversed phase HPLC (C18-silica gel, eluting with water and acetonitrile) gave the title compound as white solids (6.6 mg). HR-MS (ES, m/z) calculated for C36H47N6O4Cl2 [(M+H)+] 697.3031, observed 697.3027.

WORKUP

后处理

  1. concentrationconcentrated
  2. customPurification of the crude residue
  3. washby reversed phase HPLC (C18-silica gel, eluting with water and acetonitrile)