HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → 4-(4-bromo-1-methyl-1H-pyrazol-5-yl)-5-chloro-2-thiophenecarboxylic acid
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 5-chloro-4-(1-methyl-1H-pyrazol-5-yl)thiophene-2-carboxylic acid | HCID 57826389 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 4-(4-bromo-1-methyl-1H-pyrazol-5-yl)-5-chloro-2-thiophenecarboxylic acid | HCID 57826444 | 79% |
Reaction Steps
A solution of 5-chloro-4-(1-methyl-1H-pyrazol-5-yl)-2-thiophenecarboxylic acid (50 mg, 0.21 mmol)[prepared in Example 95] and NBS (36.7 mg, 0.21 mmol) in tetrahydrofuran (2.06 ml) was stirred in a sealed tube for 1 h at 70° C. The reaction mixture was then partitioned between H2O-DCM and the aqueous phase was washed several times with DCM. The combined organic fractions were dried over Na2SO4 and concentrated yielding 4-(4-bromo-1-methyl-1H-pyrazol-5-yl)-5-chloro-2-thiophenecarboxylic acid (82 mg, 0.16 mmol, 79% yield) as a yellow oil: LCMS (ES) m/e 257, 259 (M, M+2)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410158B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-c9b84cc808f7443f9b1b414116aaf705 |
| Source note | uspto-grants-2013_04 |