HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo- 1H-purin-8-yl)ethenyl)phenoxy)-, ethyl ester, (E)-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl chloroacetate | HCID 7751 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 1H-Purine-2,6-dione, 3,7-dihydro-1,3-diethyl-8-(2-(4-hydroxyphenyl)eth enyl)-7-methyl-, (E)- | HCID 135665343 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Acetic acid, (4-(2-(1,3-diethyl-2,3,6,7-tetrahydro-7-methyl-2,6-dioxo- 1H-purin-8-yl)ethenyl)phenoxy)-, ethyl ester, (E)- | HCID 6448954 | 91% |
Reaction Steps
Compound 175 (300 mg, 0.88 mmol) obtained in Reference Example 114 was dissolved in 10 ml of dimethylformamide. To the solution were added 731 mg (5.29 mmol) of potassium carbonate and 0.47 ml (4.41 mmol) of ethyl chloroacetate, and the mixture was stirred at room temperature for 2 hours. Water was added thereto to dissolve potassium carbonate and the deposited crystals were collected by filtration. The collected crude crystals were dissolved in chloroform, washed with a saturated aqueous solution of sodium chloride and dried over anhydrous sodium sulfate, followed by evaporation under reduced pressure. The residue was recrystallized from hexane/ethyl acetate to give 341 mg (yield 91%) of Compound 180 as pale yellow needles.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05484920 |
| Source dataset | uspto-grants-1996_01 |
| ORD ID | ord-2a1aee767db54290b2172071cad6cd9d |
| Source note | uspto-grants-1996_01 |