HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 22707380, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Chloride | HCID 5234 | — |
| Reactant | Ethyl isothiocyanate | HCID 10966 | — |
| Reactant | HCID 11223943 | HCID 11223943 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22707380 | HCID 22707380 | 29% |
Reaction Steps
To a solution of 502.5 mg (1.19 mmol) of 4-(6-amino-7-ethylamino-4-quinazolinyl)-N-benzyl-1-piperazinethiocarboxamide obtained in Example 461 in 10 ml of dimethylformamide was added 0.10 ml (1.19 mmol) of ethyl isothiocyanate, followed by overnight stirring at room temperature. To the resulting mixture was added 0.10 ml (1.19 mmol) of ethyl isothiocyanate, followed by heating at 80° C. with stirring for 4 hours. The reaction mixture was allowed to cool to room temperature, and then poured into water, and sodium chloride was added thereto. The precipitated crystals were collected by filtration, washed with water, and dried, followed by purification by silica gel chromatography to give the desired compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06472391B2 |
| Source dataset | uspto-grants-2002_10 |
| ORD ID | ord-2510782be9b44fe8abbd7f33fb55cd3f |
| Source note | uspto-grants-2002_10 |