HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → HCID 57025095, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Hydrazine hydrate (1:1) | HCID 24654 | — |
| Reactant | 4-Chloro-2-(methylthio)thieno[3,2-d]pyrimidine | HCID 1481007 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 57025095 | HCID 57025095 | 93% |
Reaction Steps
4-Chloro-2-methylthiothiopheno[3,2-d]pyrimidine (15.26 g, 70.4 mmol) was mixed with 400 mL of ethanol and then 7.2 mL (148 mmol) of hydrazine hydrate was added with stirring at ambient temperature and the mixture was allowed to stir overnight. The solid materials present were recovered by filtration and the filtrate was evaporated to dryness under reduced pressure to obtain additional solid material. All of the solids were combined and mixed vigorously with a mixture of 500 mL of dichloromethane and 500 mL of water for 6 hours. The solids present were recovered by filtration and dried to obtain 13.9 g of the title compound as a slightly yellow solid melting at 242°-244° C. The proton NMR spectrum was consistent with the assigned structure.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05494887 |
| Source dataset | uspto-grants-1996_02 |
| ORD ID | ord-14eacbc857a04b19bba5a11342760ece |
| Source note | uspto-grants-1996_02 |