HuagongsheHuagongshe Chemistry Print Report · For research reference only
Butyl chloroformate → HCID 10184083, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Butyl chloroformate | HCID 61140 | — |
| Reactant | HCID 66775157 | HCID 66775157 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Triethylamine | HCID 8471 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 10184083 | HCID 10184083 | 9.2% |
Reaction Steps
59 mg (0.16 mmol) of the crude 3-(4-[1,2,4]triazol-1-ylmethylphenyl)-5-iso-butylthiophene-2-sulfonamide from step (c) above was mixed with butyl chloroformate (31 μL, 0.24 mmol) and 4-dimethylaminopyridine (2 mg, 16 μmol) in 5 mL of triethylamine at 0° C. The reaction mixture was stirred overnight and then diluted with ethyl acetate, washed with water and dried over K2CO3. The reaction mixture was then separated on a silica column (dichloromethane+15% methanol), circular chromatography (dichloromethane+10-15% methanol and preparative LC-MS to yield 7.0 mg of the title compound (9% isolated yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07652054B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-d3e3e7a879844d1eb71a5ab14dfaaa71 |
| Source note | uspto-grants-2010_01 |