HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trichloroacetyl chloride → HCID 178511092, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trichloroacetyl chloride | HCID 6420 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Acetonitrile--water (1/1) | HCID 18373917 | — |
| Reactant | HCID 178513882 | HCID 178513882 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178511092 | HCID 178511092 | — |
Reaction Steps
To a solution of 3-cyclopentyl-3-[4-(2-hydroxy-5-oxo-6,7-dihydro-5H-pyrrolo[2,3-d]pyrimidin-4-yl)-1H-pyrazol-1-yl]propanamide (0.006 g, 0.02 mmol) in methylene chloride (0.5 mL) containing triethylamine (20 TL, 0.2 mmol) was added trichloroacetyl chloride (20 TL, 0.2 mmol). When the reaction was complete, preparative HPLC-MS (MeCN/H2O containing 0.15% NH4OH) was used to afford purified product (3 mg, 52%). 1H NMR (400 MHz, d6-DMSO): δ 11.39 (br s, 1H), 9.37 (s, 1H), 8.77 (s, 1H), 8.63 (s, 1H), 4.68-4.59 (m, 1H), 3.94 (s, 2H), 3.19-3.15 (m, 2H), 2.42-2.30 (m, 1H), 1.86-1.75 (m, 1H), 1.69-1.20 (m, 6H), 1.18-1.05 (m, 1H); LCMS (M+H)+: 339.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08486902B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-6fc1c005147e441ebccdc4057355899a |
| Source note | uspto-grants-2013_07 |