HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobutyryl chloride → 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | 3,4-dihydrothieno[3,2-f][1,4]thiazepin-5(2H)-one | HCID 4365942 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one | HCID 21472056 | 59% |
Reaction Steps
To a mixture of 13 g of 2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one and 21.5 g of 4-chlorobutyryl chloride in 200 ml of dichloroethane was added 21.5 g of aluminum chloride under cooling and the mixture was stirred for 3 hours. The mixture was poured into ice-cold water and extracted with chloroform. The organic layer was washed with saline solution, dried over magnesium sulfate and concentrated. The residue was recrystallized from ethanol to give 12 g of 7-(4-chlorobutyryl)-2,3-dihydrothieno[3,2-f][1,4]thiazepin-5(4H)-one as white crystals, m.p. 124°-125° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05691330 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-4fe21fffeb3b499886d0dd311c14643d |
| Source note | uspto-grants-1997_11 |