HuagongsheHuagongshe Chemistry Print Report · For research reference only
Toluene → HCID 70565200, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 70564203 | HCID 70564203 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 70565200 | HCID 70565200 | 97.6% |
Reaction Steps
4-Fluorobenzothiazolone (4.23 g, 0.025 mole) was dissolved in a solution of sodium hydroxide (1.60 g, 0.0375 mole) in water (100 c.c.), and tetra-n-butylammonium bromide (0.24 g, 7.5×10-4 mole) and toluene (40 c.c.) were added thereto. Dimethyl sulfate (4.70 g, 0.0375 mole) was added dropwise thereto at room temperature, and the mixture was stirred at room temperature for 1 hour, followed by phase-separation. The toluene layer was washed once with water, and the solvent was removed under reduced pressure to obtain 4.47 g of 4-fluoro-N-methylbenzothiazolone as white crystals. Yield 97.6%, purity 98.7%, m.p. 121.5°-123.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04293702 |
| Source dataset | uspto-grants-1981_10 |
| ORD ID | ord-17117c528c6e478495ab26532c5c39bd |
| Source note | uspto-grants-1981_10 |