Water → HCID 178440032, compound

HRID 267196Notes

Reaction equation

HRID 267196 reaction equation
Cl.[NH2:2][C:3]1[NH:8][C:7](=O)[C:6]2=[C:10]([CH3:16])[N:11]=[C:12]([CH2:13][CH2:14][CH3:15])[N:5]2[N:4]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[NH2:2][C:3]1[NH:8][CH2:7][C:6]2=[C:10]([CH3:16])[N:11]=[C:12]([CH2:13][CH2:14][CH3:15])[N:5]2[N:4]=1

Participants

6

Reactant 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 137220065HCID 137220065, compound

Product 1

HCID 178440032HCID 178440032, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

2-Amino-5-methyl-7-propylimidazo[5,1-f]-as-triazin-4(3H)-one, hydrochloride (5 g.) (prepared according to Example 8 of application Ser. No. 300,749 and lithium aluminium hydride (2.9 g.) in tetrahydrofuran were heated under reflux for 78 hours, and cooled. Water (11.6 ml.) was added cautiously followed by aqueous sodium hydroxide (2.9 ml., 15%). The solid was filtered off, the filtrate was evaporated and the residue was triturated with ethyl acetate. The product was crystallised from ethyl acetate and had m.p. 242°-246°.

Workup

  1. temperatureunder reflux for 78 hours
  2. temperaturecooled
  3. filtrationThe solid was filtered off
  4. customthe filtrate was evaporated
  5. customthe residue was triturated with ethyl acetate
  6. customThe product was crystallised from ethyl acetate

Sources & evidence

ORD record
ord-5295de0693be4b319ad3d3a81b361e2b
Source dataset
uspto-grants-1976_03
Patent number
US03941785

Reaction notes

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