HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,6-Di-tert-butyl-4-methylpyridine → tert-butyl ({[(1R,2S,4R)-4-({6-[(1S)-2,3-dihydro-1H-inden-1-ylamino]pyrimidin-4-yl}amino)-2-hydroxycyclopentyl]methoxy}sulfonyl)carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,6-Di-tert-butyl-4-methylpyridine | HCID 98898 | — |
| Reactant | tert-butyl N-(chlorosulfonyl)carbamate | HCID 15677406 | — |
| Reactant | HCID 66797896 | HCID 66797896 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | tert-butyl ({[(1R,2S,4R)-4-({6-[(1S)-2,3-dihydro-1H-inden-1-ylamino]pyrimidin-4-yl}amino)-2-hydroxycyclopentyl]methoxy}sulfonyl)carbamate | HCID 86618704 | 33% |
Reaction Steps
A neat mixture of (1S,2R,4R)-4-({6-[(1S)-2,3-dihydro-1H-inden-1-ylamino]pyrimidin-4-yl}amino)-2-(hydroxymethyl)cyclopentanol (100. mg, 0.294 mmol) and 2,6-di-tert-butyl-4-methylpyridine (181 mg, 0.881 mmol) was dissolved in ACN (5.00 mL) before tert-butyl (chlorosulfonyl)carbamate (95.0 mg, 0.441 mmol, as prepared in Example 21c) was added. The reaction was stirred for 2 h before being quenched via addition of MeOH (2 mL). The resulting mixture was concentrated in vacuo and purified via silica gel chromatography eluting with a gradient of 10 to 20% MeOH in DCM to afford the title compound as an amorphous solid (50.0 mg, 33%). LC/MS: Rt=1.24 min, ES+ 520. (AA standard).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08481550B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-e96e200f64c9480bb21744f094b52245 |
| Source note | uspto-grants-2013_07 |