HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 707595Generated: October 30, 2026
Benzyl chloroformate → HCID 66602125, compound
https://huagongshe.com/reaction/707595
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (6s)-6-(4-Cyano-2-Methylsulfonyl-Phenyl)-4-Methyl-2-Oxidanylidene-3-[3-(Trifluoromethyl)phenyl]-1,6-Dihydropyrimidine-5-Carbonitrile | HCID 42642360 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 66602125 | HCID 66602125 | 46% |
Reaction Steps
The reaction was carried out under argon. (4S)-4-[4-Cyano-2-(methylsulfonyl)phenyl]-6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2,3,4-tetrahydropyrimidine-5-carbonitrile (115 mg, 250 μmol) was initially charged in dry THF (3 ml), and sodium hydride (60% in mineral oil; 14 mg, 350 μmol; 1.4 eq.) was added at 0° C. The mixture was warmed to RT and stirred for 20 min. A solution of benzyl chloroformate (60 mg, 350 μmol; 1.4 eq.) in THF (1 ml) was then slowly added dropwise. After a reaction time of 1.5 h, the reaction mixture was concentrated and the crude product was purified by preparative HPLC (column: Gromsil C-18 10 μm; mobile phase: acetonitrile/water+0.1% TFA 10:90→90:10). This gave the title compound as a colorless solid (68 mg, 46% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09174997B2 |
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| Source dataset | uspto-grants-2015_11 |
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| ORD ID | ord-1ef1484bc62047e0b159904efd0ee029 |
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| Source note | uspto-grants-2015_11 |
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