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HRID2088150

反应详情

EQUATION

反应方程式

HRID 2088150 的结构方程式

REACTANTS

反应物

3
结构：CI
HCID6328

Methyl iodide

CH3I

结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：O[C@H]1C[C@@]2(c3ccccc3)[C@H](OCc3cc(C(F)(F)F)cc(C(F)(F)F)c3)CC[C@@H]1N2Cc1ccccc1
HCID86586680

未命名化合物

PRODUCTS

生成物

1
结构：CO[C@H]1C[C@@]2(c3ccccc3)[C@H](OCc3cc(C(F)(F)F)cc(C(F)(F)F)c3)CC[C@@H]1N2Cc1ccccc1
HCID86586682

未命名化合物

收率 75%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

PROCEDURE

实验过程

A mixture of (1R*,2R*,5S*,6S*)-8-benzyl-2-{[3,5-bis(trifluoromethyl)phenyl]methoxy}-1-phenyl-8-azabicyclo[3.2.1]octan-6-ol (Example 43; 22 mg 0.041 mmol), methyl iodide (0.5 ml), sodium hydride (40 mg, 1 mmol) and THF (2 ml) was stirred at room temperature for 24 hours, quenched quenched with saturated aqueous NH4Cl and extracted into dichloromethane. The combined organic extracts were dried (Na2SO4) and concentrated. The residue was purified by preparative TLC on silica gel (iso-hexane:diethyl ether 30%) to give the title compound (17 mg, 75%).

WORKUP

后处理

  1. customquenched
  2. customquenched with saturated aqueous NH4Cl
  3. extractionextracted into dichloromethane
  4. dry with materialThe combined organic extracts were dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue was purified by preparative TLC on silica gel (iso-hexane:diethyl ether 30%)