Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 67085175 | HCID 67085175 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 67085325 | HCID 67085325 | 100.3% |
Reaction Steps
The compound of formula (XIII) obtained in Example 2-1 (60 g, 97.9 mmol) was mixed with DMSO (36 ml) and methylene chloride (300 ml). The resulting solution was cooled to 0° C. and N,N-diisopropylethylamine (DIPEA) (59.7 ml, 0.343 mol) was added thereto, followed by adding a mixture solution of pyridine.SO3 complex (31.2 g), pyridine (15.9 ml) and DMSO (36 ml). The mixture thus obtained was stirred for 30 min. After completion of the reaction, the organic layer thus obtained was washed with saturated ammonium chloride (300 ml), 2M HCl solution (300 ml), sodium bicarbonate solution (300 ml) and brine (300 ml) respectively, dried over anhydrous sodium sulfate, filtered, and condensed under a reduced pressure to obtain the title compound (60 g, yield: 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08569491B2 |
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| Source dataset | uspto-grants-2013_10 |
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| ORD ID | ord-74f4ad0da718455d9f27ddd50f18ecda |
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| Source note | uspto-grants-2013_10 |
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