HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylene Glycol → 1-(8-Chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylene Glycol | HCID 174 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1-Carbethoxy-4-(8-chloro-10,11-dihydro-2-methyl-dibenzo[b,f]-thiepin-10-yl)piperazine | HCID 21416091 | — |
| Solvent | Water | HCID 962 | — |
| Product | 1-(8-Chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)piperazine | HCID 21416163 | — |
Reaction Steps
95 G. of 1-carbethoxy-4-(8-chloro-10,11-dihydro-2-methyl-dibenzo[b,f]thiepin-10-yl)-piperazine are stirred together with 1,000 ml. of ethyleneglycol, 77 g. of potassium hydroxide and 10 ml of water on a bath of 160° for 6 hours. The reaction mixture is poured over ice water and extracted with ether. The ether extract is washed with water, dried and evaporated, whereby 1-(8-chloro10,11-dihydro-2-methyl-dibenzo[b,f]-thiepin-10-yl)-piperazine is obtained as a red-brown viscous oil. After recrystallization from acetone/petroleum ether the product is obtained as crystals having a melting point of 125°-127°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04044010 |
| Source dataset | uspto-grants-1977_08 |
| ORD ID | ord-86c209f8ba024c468807975b707260f3 |
| Source note | uspto-grants-1977_08 |