HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chlorobutyryl chloride → HCID 21471973, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chlorobutyryl chloride | HCID 78370 | — |
| Reactant | Aluminum(III) Chloride | HCID 6451240 | — |
| Reactant | HCID 21471960 | HCID 21471960 | — |
| Solvent | 1,1-Dichloroethane | HCID 6365 | — |
| Product | HCID 21471973 | HCID 21471973 | 15.2% |
Reaction Steps
To a mixture of 5 g of 2-methyl-5,6,7,8-tetrahydro-4H-thieno[3,2-c]azepin-4-one and 5 g of 4-chlorobutyryl chloride in 50 ml of dichloroethane was added 8.6 g of aluminum chloride under ice-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 1.2 g of 3-(4-chlorobutyryl)-2-methyl-5,6,7,8-tetrahydro-4H-thieno[3,2-c]azepin-4-one as white crystals, m.p. 113°-115° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05532240 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-68489657fd1a4c4699028b322d42078b |
| Source note | uspto-grants-1996_07 |