Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Cysteamine Hydrochloride | HCID 9082 | — |
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | 2-Ethylhexanoyl chloride | HCID 79103 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 59403792 | HCID 59403792 | — |
Reaction Steps
22.7 g of 2-mercaptoethylamine hydrochloride (0.2 mol) and 32.4 g of triethylamine (0.32 mol) were introduced in suspension in 130 ml of dichloromethane at 0° C.-5° C. Over the course of 25 minutes, 16.8 g of 2-ethylhexanoyl chloride (0.1 mol) were added dropwise. The batch was stirred at 0° C. to 5° C. for 1 hour, at 40° C. for 1.5 hours, and then at room temperature for 12 hours. 70 ml of saturated ammonium chloride solution were added and a phase separation was carried out. This was repeated twice and the organic phases were combined, dried over sodium sulfate, and freed of their solvent under reduced pressure. The residue obtained was purified by column chromatography (97 toluene:3 methanol).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08460445B2 |
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| Source dataset | uspto-grants-2013_06 |
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| ORD ID | ord-119ec1ba758c4225907bdb84a474019c |
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| Source note | uspto-grants-2013_06 |
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