Ammonia → HCID 178509082, compound
Reaction equation
[NH3:1].[Cl:2][C:3]1[CH:12]=[CH:11][C:10]2[N:9]=[C:8](SC)[N:7]3[N:15]=[C:16]([C:18]4[O:19][CH:20]=[CH:21][CH:22]=4)[N:17]=[C:6]3[C:5]=2[CH:4]=1>[OH-].[NH4+]>[Cl:2][C:3]1[CH:12]=[CH:11][C:10]2[NH:9][C:8](=[NH:1])[N:7]3[N:15]=[C:16]([C:18]4[O:19][CH:20]=[CH:21][CH:22]=4)[N:17]=[C:6]3[C:5]=2[CH:4]=1Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of concentrated aqueous ammonium hydroxide (300 ml) saturated with ammonia gas at 0° and 9-chloro-2-(2-furyl)-5-methylthio[1,2,4]triazolo[1,5-c]quinazoline (5.7 g) in a stainless steel pressure vessel is heated at an outside temperature of 150° over 18 hours, during which time the pressure rises to 250 p.s.i. The reaction mixture is cooled and the solid material collected, washed with water and air dried. The 9-chloro-2-(2-furyl)-5-imino-5,6-dihydro-[1,2,4]triazolo[1,5-c]quinazoline thus obtained (2.9 g, mp 269°-271°) is converted to the methanesulphonate salt by dissolution in 2-methoxyethanol (150 ml) followed by methanesulphonic acid (0.66 ml) and dry ether (25 ml) to afford the pure salt identical to that from Example 32.
Workup
- temperatureThe reaction mixture is cooled
- customthe solid material collected
- washwashed with water and air
- customdried
Sources & evidence
- ORD record
- ord-6c755ca033fd4be1ac8eb1032d5cda7e
- Source dataset
- uspto-grants-1987_12
- Patent number
- US04713383
Reaction notes
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