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HRID244920

反应详情

EQUATION

反应方程式

HRID 244920 的结构方程式

REACTANTS

反应物

2
结构：O=C(O)C(F)(F)F
HCID6422

未命名化合物

结构：COC(=O)c1sc(C#CC(C)(C)C)cc1N(C(=O)[C@H]1CC[C@H](C)CC1)C1CCN(C(=O)OC(C)(C)C)CC1
HCID178499336

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)c1sc(C#CC(C)(C)C)cc1N(C(=O)[C@H]1CC[C@H](C)CC1)C1CCNCC1
HCID178499334

未命名化合物

收率 125.9%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

2 次

PROCEDURE

实验过程

The product from step IV (5.198 g) is dissolved in 30 mL of CH2Cl2 and treated with 20 mL of trifluoroacetic acid. The mixture is stirred at room temperature overnight, then it is evaporated to dryness, obtained residue is redissolved in CH2Cl2 and washed with aqueous NaHCO3 and brine. Organic fraction is separated, dried over Na2SO4, and concentrated to give 5.340 g of crude 5-(3,3-dimethyl-but-1-ynyl)-3-[(trans-4-methyl-cyclohexanecarbonyl)-(piperidin-4-yl)amino]-thiophene-2-carboxylic acid methyl ester.

WORKUP

后处理

  1. customit is evaporated to dryness
  2. customobtained residue
  3. washwashed with aqueous NaHCO3 and brine
  4. customOrganic fraction is separated
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated