Hydride → 1-二苯基甲基-3-氮杂啶乙胺

HRID 872

反应方程式

HRID 872 反应方程式
[C:1]([CH2:3][CH:4]1[CH2:7][N:6]([CH:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)[CH2:5]1)#[N:2].[H-].[H-].[H-].[H-].[Li+].[Al+3].[H-]>C1COCC1>[NH2:2][CH2:1][CH2:3][CH:4]1[CH2:7][N:6]([CH:8]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[C:9]2[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=2)[CH2:5]1

参与物

5

反应物 3

HCID 166653HydrideHCID 21226445Aluminium lithium hydrideHCID 222576333-Cyanomethyl-1-benzhydryl azetidine

产物 1

HCID 222576341-二苯基甲基-3-氮杂啶乙胺收率 87%

试剂、催化剂与溶剂 1

HCID 8028四氢呋喃溶剂

实验过程

5.7 g (21.7 mmol) of 3-cyanomethyl-1-benzhydryl azetidine was added slowly to a suspension of 2.9 g (76.0 mmol) of LiAlH4 in 80 mL of dry THF at roomtemperature. The reaction mixture was refluxed for 4 h. Excess hydride reagent was hydrolyzed by careful addition, with cooling, of NH4 Cl(aq), the gelatinous mixture was filtered and the filter cake was washed repeatedly with THF. The solvent was evaporated, the residue was dissolved in diethyl ether, washed with brine and dried with Na2SO4. Evaporation of the solvent gave 5.0 g (87%) of the title compound.

后处理

  1. temperatureThe reaction mixture was refluxed for 4 h
  2. filtrationthe gelatinous mixture was filtered
  3. washthe filter cake was washed repeatedly with THF
  4. customThe solvent was evaporated
  5. dissolutionthe residue was dissolved in diethyl ether
  6. washwashed with brine
  7. dry with materialdried with Na2SO4
  8. customEvaporation of the solvent

来源与证据

ORD记录
ord-df1a0a7ecbb7442b9ee9a9bf29ebf6f4
来源数据集
uspto-grants-1998_03
专利号
US05723444

关联笔记

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