HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Nitrobenzoyl chloride → HCID 59774863, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Nitrobenzoyl chloride | HCID 8502 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 59774920 | HCID 59774920 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59774863 | HCID 59774863 | 96.5% |
Reaction Steps
To a 0° C. solution of crude 3-(trifluoromethyl)-1-(triisopropylsilyl)hex-5-en-1-yn-3-ol from Step 1 (242 mg, 0.755 mmol) in DMF (2 mL) was added NaH (60% disp., 32 mg, 0.793 mmol) in two portions. The mixture was allowed to reach room temperature and stirred for 40 min. A solution of 4-nitrobenzoyl chloride (147 mg, 0.793 mmol) in DMF (1 mL) was added dropwise. After 1.5 h, the mixture was poured in H2O and extracted with EtOAc (3×). The combined organic layers were washed with H2O (3×) and brine, dried (Na2SO4) and concentrated, affording the title compound (342 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07960409B2 |
| Source dataset | uspto-grants-2011_06 |
| ORD ID | ord-2060469509be43139097706ff72b8386 |
| Source note | uspto-grants-2011_06 |