HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → HCID 15280235, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | 8-Chloro-5,11-dihydro[1]benzothiepino[4,3-b]pyridin-11-ol | HCID 15280234 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15280235 | HCID 15280235 | 84.9% |
Reaction Steps
Add thionyl chloride (3.1 mL, 0.0425 mol) dropwise to a stirred suspension of 8-chloro-5,11-dihydro[1]benzothiepino[4,3-b]pyridin-11-ol (8.8 g, 0.0334 mol) in CH2Cl2 (75 mL) at 3°-8° C. Stir the mixture at room temperature for 3 hours, and pour it into 150 mL of 2.5M NaOH containing ice. Filter, separate the aqueous layer and extract it with CH2Cl2 (2×50 mL). Combine the organic extracts, and wash with water (3×50 mL) and brine (1×75 mL). Dry the mixture over MgSO4, filter, and concentrate in vacuo to obtain the title compound (8.0 g, 80%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05430032 |
| Source dataset | uspto-grants-1995_07 |
| ORD ID | ord-74fff8fe7ccb48b6b5c0bb970c335fc6 |
| Source note | uspto-grants-1995_07 |