HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 66656291, compound → HCID 56602346, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 66656291 | HCID 66656291 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Pyridinium chloride | HCID 10176127 | — |
| Product | HCID 56602346 | HCID 56602346 | 41.5% |
Reaction Steps
Heat a solution of 5-(1-trityl-1H-pyrazol-4-yl)-thiophene-2-carboxylic acid 3-(2-methyl-1,2,3,4-tetrahydro-isoquinolin-7-ylcarbamoyl)-benzylamide (167 mg, 0.234 mmol) in 10% pyridine/HCl in MeOH (50 mL) at 50° C. overnight. Cool the reaction to rt, concentrate, and purify the residue by prep-HPLC (10% to 90%, CH3CN/water). Further purify the residue through a short silica plug to remove baseline impurity affording desired product 5-(1H-pyrazol-4-yl)-thiophene-2-carboxylic acid 3-(2-methyl-1,2,3,4-tetrahydro-isoquinolin-7-ylcarbamoyl)-benzylamide (68 mg, 0.097 mmol). MS, electrospray 472.2 (M+H), rt 0.94 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697911B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-80173193bf8141b59a614c4df2b299cd |
| Source note | uspto-grants-2014_04 |