HuagongsheHuagongshe Chemistry Print Report · For research reference only
3,4-Dichloroaniline → HCID 178526426, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3,4-Dichloroaniline | HCID 7257 | — |
| Reactant | HCID 178526425 | HCID 178526425 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 178526426 | HCID 178526426 | 100% |
Reaction Steps
A solution of 8-bromo-2-chloro-6-nitroquinazolin-4-ol (2.96 g) and 3,4-dichloroaniline (4.72 g) in 1-methyl-2-pyrrolidinone (70 mL) was heated at 140° C. for 3 h. The mixture was cooled to room temperature and poured onto ice/water (600 mL). The precipitate which formed was filtered, washed with water (50 mL), diethyl ether (150 mL) and dried in vacuo to afford the title compound (4.18 g). 1H NMR (300 MHz, DMSO-d6) δ11.62 (s, 1H), 9.64 (s, 1H), 8.72-8.65 (m, 3H), 7.61 (s, 1H), 7.60 (5, 1H); HPLC (Method B): 10.56 min. MS (APCI−): m/z 429, 431.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06399603B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-a5b8b677cdad4cc288f7017ba95202a1 |
| Source note | uspto-grants-2002_06 |