Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 19972525 | HCID 19972525 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 19972408 | HCID 19972408 | — |
Reaction Steps
53.4 g of Intermediate II and 38.8 ml of anhydrous triethylamine were dissolved in 440 ml of chloroform. A solution of 19.8 ml of thionyl chloride in 80 ml of anhydrous chloroform was added to the above solution, which was maintained at -10°/-2° C. The reaction mixture was stirred at ambient temperature for 4 hours, and then diluted with 400 ml of water. The aqueous phase was extracted with chloroform, and the extracts were added to the chloroform phase. The chloroform solution was washed with brine, dried on anhydrous sodium sulphate and evaporated to dryness in vacuo. Yield: 56 g of the title compound, which, recrystallized from ethanol, has a melting point of 112°-113° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05453518 |
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| Source dataset | uspto-grants-1995_09 |
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| ORD ID | ord-9547ec1c253b44c490ece97fba9a43be |
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| Source note | uspto-grants-1995_09 |
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