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HRID1190013

反应详情

EQUATION

反应方程式

HRID 1190013 的结构方程式

REACTANTS

反应物

2
结构：Cl
HCID313

Hydrochloric Acid

ClH

结构：C[C@H]1CC[C@H](C(=O)N(c2cc(C3=CCC4(CC3)OCCO4)sc2C(=O)O)[C@H]2CC[C@H](O)CC2)CC1
HCID178461267

未命名化合物

PRODUCTS

生成物

1
结构：C[C@H]1CC[C@H](C(=O)N(c2cc(C3=CCC(=O)CC3)sc2C(=O)O)[C@H]2CC[C@H](O)CC2)CC1
HCID178461279

未命名化合物

收率 71.2%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：ClCCl
溶剂HCID6344

Dichloromethane

CH2Cl2

结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

To a solution of 5-(1,4-Dioxa-spiro[4.5]dec-7-en-8-yl)-3-[(trans-4-hydroxy-cyclohexyl)-(trans-4-methyl-cyclohexanecarbonyl)-amino]-thiophene-2-carboxylic acid (428 mg, 0.85 mmol) in THF (5 mL) was added 3N HCl (2.5 mL), and the mixture was heated at 40° C. for 5 h. Then it was diluted with CH2Cl2 (70 mL) and washed with brine and water. Organic fraction was dried over Na2SO4, concentrated under reduced pressure and the residue was purified by column chromatography on silica gel eluting with 0-10% MeOH in CH2Cl2 to give 278 mg (71%) of 3-[(trans-4-hydroxy-cyclohexyl)-(trans-4-methyl-cyclohexanecarbonyl)-amino]-5-(4-oxo-cyclohex-1-enyl)-thiophene-2-carboxylic acid.

WORKUP

后处理

  1. washwashed with brine and water
  2. dry with materialOrganic fraction was dried over Na2SO4
  3. concentrationconcentrated under reduced pressure
  4. customthe residue was purified by column chromatography on silica gel eluting with 0-10% MeOH in CH2Cl2