HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21471762, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 21471822 | HCID 21471822 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21471762 | HCID 21471762 | 36.9% |
Reaction Steps
To a solution of 2 g of 4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one and 2.5 g of 4-chlorobutyryl chloride in 25 ml of dichloromethane was added 4.8 g of aluminum chloride under cooling. The mixture was stirred for 80 minutes, refluxed under heating and poured into water, and then extracted with chloroform. The extract was washed with water, dried over magnesium sulfate and concentrated. The residue was crystallized from ethyl acetate-isopropyl ether to give 1.2 g of 2-(4-chlorobutyryl)-4,5,6,7-tetrahydro-8H-thieno[2,3-c]azepin-8-one as white crystals, m.p. 163°14 165° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05691330 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-1f5f5db0934a489dad5c53cbd29881d6 |
| Source note | uspto-grants-1997_11 |