HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 19799240, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 19799247 | HCID 19799247 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19799240 | HCID 19799240 | — |
Reaction Steps
Sodium hydride (60% dispersion in oil; 196 mg) was added to a stirred solution of 8-fluoro-2,3,4,5-tetrahydro-1H-pyrido[4,3-b]indol-1-one (500 mg) in dry DMF (20 ml) at 21° under nitrogen. After 15 min, the solution was cooled (0°) and a 10% (v/v) solution of methyl iodide in DMF (1.6 ml) was added dropwise. After 10 min, water (150 ml) was added and the mixture was extracted with ethyl acetate (3×50 ml). The combined organic extracts were washed with water (3×50 ml), then brine (100 ml) and evaporated to give a solid which was purified by FCC Eluting with dichloromethane:methanol (80:1) to give the title compound (240 mg), m.p. 200°-202°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05183820 |
| Source dataset | uspto-grants-1993_02 |
| ORD ID | ord-9270dc58495541b4b6ed140e45b650d8 |
| Source note | uspto-grants-1993_02 |