HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 13922870, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Morpholine | HCID 8083 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 13922868 | HCID 13922868 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 13922870 | HCID 13922870 | 9.6% |
Reaction Steps
To a stirred solution of morpholine (0.91 g, 10.5 mmol) and triethylamine (1.01 g, 10 mmol) in 20 ml of methanol was added 5-bromomethyl-2-sulfamoylbenzo[b]thiophene (3.06 9, 10 mmol) portionwise over 5 minutes at ambient temperature. Stirring was continued for 11/4 hours. The resulting suspension was cooled and filtered after an additional 1 hour to give 2.76 g. of yellow solid. Concentration of the filtrate in vacuo followed by trituration of the residue with water and filtering gave an additional 0.3 g of yellow solid. (Total crude yield was 98%). Recrystallization from nitromethane gave material with m.p. 221.5°-224° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04668697 |
| Source dataset | uspto-grants-1987_05 |
| ORD ID | ord-4355a688628f4cb0904fd9285eb9fc92 |
| Source note | uspto-grants-1987_05 |