HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanesulfonic Acid → 8-Fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]-thiepin-10-ol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanesulfonic Acid | HCID 6395 | — |
| Reactant | (R)-1-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine | HCID 54274820 | — |
| Product | 8-Fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]-thiepin-10-ol | HCID 12275542 | — |
Reaction Steps
2.3 G. of enriched (R)-1-(8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine [αD = -25.0° (chloroform; c = 2.50%)] are heated to reflux with stirring for 24 hours in 0.57-M methanesulfonic acid and worked up in a manner analogous to that described in Example 13. For purification, the benzene extract is chromatographed on silica gel (0.2-0.5 mm) with chloroform. The eluted oily racemic 8-fluoro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-ol melts at 90.5° C. after recrystallization from n-hexane.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04089861 |
| Source dataset | uspto-grants-1978_05 |
| ORD ID | ord-8fdfe61f2a2344a1a04dd3af7ad4c19b |
| Source note | uspto-grants-1978_05 |