HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosulfonic acid → HCID 22908976, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosulfonic acid | HCID 24638 | — |
| Reactant | 141807-86-5 | HCID 6448583 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 22908976 | HCID 22908976 | 39.1% |
Reaction Steps
(E)-7-Methyl-1,3-dipropyl-8-styrylxanthine (WO92/06976) (500 mg, 1.42 mmol) was dissolved in chloroform (5 ml), and chlorosulfonic acid (0.28 ml, 4.26 mmol) was added dropwise thereto at 0° C. The resulting solution was heated under reflux for 3 hours and then poured into 20 ml of ice-water. The chloroform layer was separated and the aqueous layer was extracted 5 times with tetrahydrofuran. The combined organic layer was dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure to give 240 mg (yield 39%) of Compound 31 as a pale yellow powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05670498 |
| Source dataset | uspto-grants-1997_09 |
| ORD ID | ord-2db91da788d14521885e62a37252e57e |
| Source note | uspto-grants-1997_09 |