Aluminium lithium hydride → HCID 178511287, compound

HRID 35974Notes

Reaction equation

HRID 35974 reaction equation
[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([C:14]([NH2:16])=O)[CH2:10][CH2:9]1>O1CCCC1>[OH:7][C@H:8]1[CH2:13][CH2:12][C@H:11]([CH2:14][NH2:16])[CH2:10][CH2:9]1

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 178513955HCID 178513955, compound

Product 1

HCID 178511287HCID 178511287, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a suspension of 11.4 g (0.3 mol) lithium aluminum hydride in 500 ml anhydrous tetrahydrofuran are introduced 21.6 g (0 15 mol) solid trans-4-hydroxycyclohexanecarboxylic acid amide and heated under reflux for 24 h. After decomposition with 45 ml saturated common salt solution, it is filtered off with suction and the filtrate distilled The residue is triturated with ether and the crystals filtered off with suction. There remain 11 g of amine, i.e. 57% of theory, of the m.p. 137°-139° C.

Workup

  1. temperatureheated
  2. temperatureunder reflux for 24 h
  3. filtrationAfter decomposition with 45 ml saturated common salt solution, it is filtered off with suction
  4. distillationthe filtrate distilled The residue
  5. customis triturated with ether
  6. filtrationthe crystals filtered off with suction

Sources & evidence

ORD record
ord-690e69fd83794de38001262a7f79ae6f
Source dataset
uspto-grants-1995_05
Patent number
US05411989

Reaction notes

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