HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 10739024, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Chloro-6,7-dimethoxy-4-quinazolinamine | HCID 90235 | — |
| Reactant | HCID 86757488 | HCID 86757488 | — |
| Solvent | Isoamyl Alcohol | HCID 31260 | — |
| Product | Ammonia | HCID 222 | — |
| Product | HCID 10739024 | HCID 10739024 | 59.3% |
Reaction Steps
A mixture of 0.36 g of 4amino-2-chloro6,7-dimethoxyquinazoline, 1.08 g of (S)-N-tert-butyl-2-piperazinecarboxamide bis-(1S)-(+)-10-camphorsulfonate, prepared as described in U.S. Pat. No. 5,700,364, and 0.94 ml of diisopropylethylamine in 10 ml of isoamyl alcohol was heated at reflux for 9 h. After cooling to room temperature, the solvent was evaporated in vacuo and 50 ml of dichloromethane was added to the residue. The mixture was washed with water (3×20 ml), 5% aqueous Na2CO3 (30 ml), water (3×20 ml), dried (Na2SO4) and evaporated to dryness. The residue was purified by flash chromatography eluting with chloroform:2N methanolic ammonia 100:3 to give 0.173 g (30%) of the desired compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06303606B1 |
| Source dataset | uspto-grants-2001_10 |
| ORD ID | ord-34210192de64493bbc5e8023411876b3 |
| Source note | uspto-grants-2001_10 |