HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 9976966, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 10364000 | HCID 10364000 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 9976966 | HCID 9976966 | 61% |
Reaction Steps
A 0.7 g quantity of 3-(4-chlorobenzyl)-1-ethoxycarbonylmethyl-5,6-dimethylthieno[2,3-d]pyrimidin-2,4(1H, 3H)-dione (Compound IV-1) prepared in Reference Example 5 was dissolved in 30 ml of methanol. To the solution was added 0.3 g of sodium hydroxide dissolved in 2 ml of water. The mixture was allowed to react at 60° C. for 30 minutes, and then the reaction mixture was concentrated. Diluted hydrochloric acid was added thereto with ice-cooling to acidify the resulting solution. The solution was filtrated and the separated crystals were recrystallized from methanol, giving 0.4 g of 1-carboxymethyl-3-(4-chlorobenzyl)-5,6-dimethylthieno[2,3-d]pyrimidin-2,4(1H, 3H)-dione having m.p. of 173° to 176° C. in a yield of 61%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04898867 |
| Source dataset | uspto-grants-1990_02 |
| ORD ID | ord-afdf4b71f0a9448c98155560b6f909b9 |
| Source note | uspto-grants-1990_02 |