Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Thiophenol | HCID 7969 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Water ethylacetate | HCID 22728543 | — |
| Reactant | HCID 86586416 | HCID 86586416 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86586417 | HCID 86586417 | — |
Reaction Steps
(2R)-3-methyl-2-[(2-chlorobenzthiazol-6-sulfonyl)amino]butanoic acid methylester (0.154 mg, 0.44 mmol) prepared in a similar manner as in Example 20 was dissolved in MeCN (3 mL) and added solid K2CO3 (0.1 mg, 1.6 equi.). Thiophenol (0.055 mL, 1.2 equi.) was also added and the reaction solution was refluxed for 3 hours. When starting material was disappeared, H2O/ethylacetate (5 mL/10 mL) was added for extraction of product. The extracted product in organic phase was washed with NaCl solution, dried over MgSO4 and distilled under reduced pressure. The extracted product was crystallized with n-hexane/ethylacetate (3/1) solution to prepare the titled compound, (2R)-3-methyl-2-[(2-phenylthiobenzthiazol-6-sulfonyl)amino]butanoic acid methylester (190 mg, 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06548667B2 |
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| Source dataset | uspto-grants-2003_04 |
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| ORD ID | ord-84dfe1a54df0478d8bdbaa89e8efd643 |
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| Source note | uspto-grants-2003_04 |
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