Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diphenyl chlorophosphate | HCID 75654 | — |
| Reactant | 1-Aminoimidazolidin-2-one | HCID 181697 | — |
| Reactant | HCID 14278968 | HCID 14278968 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 14278969 | HCID 14278969 | — |
Reaction Steps
To a solution of 6,7-dimethoxy-3-isoquinolinecarboxylic acid (6.99 g, 30.0 mmol) in 300 ml of N,N-dimethylformamide were added triethylamine (12.14 g, 120.0 mmol) and diphenyl chlorophosphate (80.6 g, 30.0 mmol) at 0° C. After stirring for 4 hours at 0° C., N-amino-2-oxoimidazolidine (3.03 g, 30.0 mmol) was added, and the mixture was stirred at 0° C. overnight. Ammonium salts (2.0 g) were filtered off, and the filtrate was evaporated in vacuo. The residue was triturated with a 1:1 mixture of water and ethyl acetate. The solid was filtered off and triturated twice with water at pH 8 for 3 hours. The remaining solid was filtered off, washed with water and dried in vacuo. Yield: 4.30 g; melting point 220° C. (dec.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US04777252 |
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| Source dataset | uspto-grants-1988_10 |
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| ORD ID | ord-e31d235e44014bf1835f60c00cdd98e8 |
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| Source note | uspto-grants-1988_10 |
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