Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Potassium hydroxy sulfite | HCID 23707502 | — |
| Reactant | HCID 69983437 | HCID 69983437 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 69982908 | HCID 69982908 | 95% |
Reaction Steps
A solution of Oxone®(9.8 g, 16 mmol) in water (50 ml) was added dropwise over 15 minutes to a solution of the benzil from Step 3 (2.0 g, 63 mmol) in a methanol:tetrahydrofuran solution (2:1, 100 ml). The reaction mixture was warmed to 40° C. for 2 hours, cooled and poured into water (500 ml). The solid precipitate was filtered and air dried to give 2.0 g (95%) of desired product as a solid: mp 181-183° C. Anal. Calc'd. for C17H16O6S (MW 348.38): C, 58.61; H, 4.63; S, 9.20. Found: C, 58.55; H, 4.49; S, 9.29.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US06426360B1 |
|---|
| Source dataset | uspto-grants-2002_07 |
|---|
| ORD ID | ord-17ec604873b844389e88c149525773c1 |
|---|
| Source note | uspto-grants-2002_07 |
|---|