HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Anhydride → HCID 178474848, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Anhydride | HCID 7918 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 178462243 | HCID 178462243 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178474848 | HCID 178474848 | 13% |
Reaction Steps
To a solution of (1R)-1-{1-[trans-4-(aminomethyl)cyclohexyl]-1H-imidazo[4,5-d]thieno[3,2-b]pyridin-2-yl}ethanol bis(trifluoroacetate) (16 mg, 0.029 mmol) and triethylamine (20. μL, 0.14 mmol) in dichloromethane (1 mL) was added acetic anhydride (4.0 μL, 0.043 mmol). The mixture was stirred at room temperature for 1 h, then stripped to dryness and purified on prep-HPLC (XBridge C18 column, eluting with a gradient of acetonitrile/water containing 0.1% ammonium hydroxide, at flow rate of 60 mL/min) to give the desired product (1.4 mg, 13%). LCMS calculated for C19H25N4O2S (M+H)+: m/z=373.2. Found: 373.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09181271B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-4eddd2b1d5874f35a856e00647135377 |
| Source note | uspto-grants-2015_11 |