Aluminium lithium hydride → HCID 178442283, compound

HRID 267198Notes

Reaction equation

HRID 267198 reaction equation
[NH2:1][C:2]1[NH:7][C:6](=O)[C:5]2=[C:9]([CH3:17])[N:10]=[C:11]([CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15])[N:4]2[N:3]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-]>COCCOCCOC>[NH2:1][C:2]1[NH:7][CH2:6][C:5]2=[C:9]([CH3:17])[N:10]=[C:11]([CH2:12][CH:13]([CH3:16])[CH2:14][CH3:15])[N:4]2[N:3]=1

Participants

4

Reactant 2

HCID 21226445Aluminium lithium hydrideHCID 137220066HCID 137220066, compound

Product 1

HCID 178442283HCID 178442283, compound

Reagents, catalysts & solvents 1

HCID 8150DiglymeSolvent

Procedure

2-Amino-5-methyl-7(2-methylbutyl)imidazo[5,1-f]-as-triazin-4(3H)-one (1.7 g.) and lithium aluminium hydride (0.9 g.) in diglyme (50 ml., freshly redistilled) were stirred and heated to 100° for 4.5 hours and cooled. Water (1 ml.) was added dropwise, followed by 2N sodium hydroxide (2 ml.) and water (1 ml.). The solid was filtered off, the filtrate was evaporated and the residue was crystallised from isopropanol. The product had m.p. 207°-213° (63%). It was converted to its hydrochloride, m.p. 203°-205.5° by treating a solution in ethanol with hydrogen chloride in ether.

Workup

  1. distillation, freshly redistilled)
  2. temperatureheated to 100° for 4.5 hours
  3. temperaturecooled
  4. additionWater (1 ml.) was added dropwise
  5. filtrationThe solid was filtered off
  6. customthe filtrate was evaporated
  7. customthe residue was crystallised from isopropanol
  8. additionby treating a solution in ethanol with hydrogen chloride in ether

Sources & evidence

ORD record
ord-33ac905def264c5394ec267700fac7bd
Source dataset
uspto-grants-1976_03
Patent number
US03941785

Reaction notes

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