HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → HCID 69053645, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | HCID 22626666 | HCID 22626666 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 69053645 | HCID 69053645 | 43% |
Reaction Steps
(6-Amino-3-pyridinyl)(4-fluorophenyl)methanone (30 mg, 0.138 mmol) was dissolved in 1 ml of trifluoroacetic acid. 16 l of sulfuric acid (2.2 eq) and 50 l of Et3SiH and stirred at ambient temperature for 4 h in a closed vial. The reaction mixture was poured into water, basified with 2N sodium hydroxide and extracted into methylene chloride. Organic extract was washed with water and brine, concentrated and purified by column chromatography on silica (10 g, EtOAc/hexane 1:1) to give 12 mg of desired product (43% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07517992B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-d67c42ae3e6b453382097dabbaaad524 |
| Source note | uspto-grants-2009_04 |