HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 478668, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | HCID 478667 | HCID 478667 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | HCID 478668 | HCID 478668 | 75% |
Reaction Steps
A solution of 8-fluoro-9-(3-methyl-4-t-butyloxycarbonylpiperazinyl)-indolo[2,1-b]quinazoline-6-12-dione (0.19 g, 0.4 mmol) (from Example 53) in methylene chloride (7 mL) and trifluoroacetic acid (7 mL) was stirred for 1 h. Chloroform was added and the chloroform/methylene chloride solution was washed with saturated sodium bicarbonate. The organic layer was separated, dried and concentrated to give a solid. Purification of the crude product by silica gel chromatography (chloroform eluent) gave the title compound in 75% yield: mp 225°-227° C.; 1H NMR (300 MHz, CDCl3) δ 8.40 (d, 1H), 8.18 (d, 1H), 8.03 (d, 1H), 7.85 (t, 1H), 7.65 (t, 1H) 7.50 (d, 1H), 4.3 (m, 1H), 3.86-3.76 (m, 2H), 3.13-3.04 (m, 4H), 2.8 (t, 1H) 1.75 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05441955 |
| Source dataset | uspto-grants-1995_08 |
| ORD ID | ord-dd05a6917a324e0495d6bb20a9b05f04 |
| Source note | uspto-grants-1995_08 |