Ethyl orthoformate → HCID 178479638, compound
Reaction equation
[ClH:1].Cl.[NH2:3][CH2:4][C:5]([C:7]1[N:8]=[CH:9][NH:10][C:11]=1[NH2:12])=[O:6].[CH:13](OCC)(OCC)OCC>C(O)C>[ClH:1].[N:8]1[C:7]2[C:5](=[O:6])[CH2:4][NH:3][CH:13]=[N:12][C:11]=2[NH:10][CH:9]=1Participants
4
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Procedure
A mixture of 285 mg. of 2-amino-1-(5-amino-1H-imidazol-4-yl)ethanone dihydrochloride (Example 1), 200 ml. of absolute ethanol and 10 ml. of triethyl orthoformate is stirred and heated at reflux for 1 hour, then cooled and evaporated at reduced pressure. The residue of 6,7-dihydroimidazo[4,5-d][1,3]diazepin-8(3H)-one monohydrochloride, which crystallizes on standing, is collected by filtration, washed with ethanol, then with ether, and dried at reduced pressure; m.p. above 250° C. dec.
Workup
- additionA mixture of 285 mg
- temperatureheated
- temperatureat reflux for 1 hour
- temperaturecooled
- customevaporated at reduced pressure
- customThe residue of 6,7-dihydroimidazo[4,5-d][1,3]diazepin-8(3H)-one monohydrochloride, which crystallizes on standing
- filtrationis collected by filtration
- washwashed with ethanol
- dry with materialwith ether, and dried at reduced pressure
Sources & evidence
- ORD record
- ord-e868e6faef424bc2be4a5bd1a4e3f28a
- Source dataset
- uspto-grants-1978_09
- Patent number
- US04117229
Reaction notes
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