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HRID862125

反应详情

EQUATION

反应方程式

HRID 862125 的结构方程式

REACTANTS

反应物

3
结构：O=S(=O)([O-])[O-].[Na+].[Na+]
HCID24436

Sodium sulfate anhydrous

Na2O4S

结构：[Al+3].[H-].[H-].[H-].[H-].[Li+]
HCID21226445

未命名化合物

结构：COc1ccc(OC)c(CN[C@H]2[C@H]3CCN([C@@H](C(=O)N(C)C)C3)[C@H]2C(c2ccccc2)c2ccccc2)c1
HCID70114647

未命名化合物

PRODUCTS

生成物

1
结构：COc1ccc(OC)c(CN[C@@H]2[C@@H]3CCN([C@H](CO)C3)[C@@H]2C(c2ccccc2)c2ccccc2)c1
HCID54206645

未命名化合物

AUXILIARIES

试剂、催化剂与溶剂

1
结构：C1CCOC1
溶剂HCID8028

Tetrahydrofuran

C4H8O

2 次

PROCEDURE

实验过程

Into a suspension of lithium aluminum hydride (LiAlH4) (92 mg, 2.4 mmole) in dry THF (10 ml) at 0° C. was added a solution of compound 35 (417 mg, 0.8 mmole) in dry THF (10 ml) and heated at reflux for 1 hour. Na2SO4 /10H2O was added to the reaction mixture and stirred for 30 minutes. After cooling, the solids were removed by filtration and washed with THF. The filtrate was evaporated, added excess 10% HCl/MeOH and concentrated down. The resulting oil was purified by recrystallization from MeOH-Ether. The white crystal was collected by filtration and dried in vacuo to give compound 41 2HCl salt (240 mg, 0.44 mmole, 55%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperatureAfter cooling
  4. customthe solids were removed by filtration
  5. washwashed with THF
  6. customThe filtrate was evaporated
  7. additionadded excess 10% HCl/MeOH
  8. concentrationconcentrated down
  9. customThe resulting oil was purified by recrystallization from MeOH-Ether
  10. filtrationThe white crystal was collected by filtration
  11. customdried in vacuo