HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroacetyl chloride → 5-Chloro-2-chloromethyl-3-o-tolyl-3H-quinazolin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroacetyl chloride | HCID 6577 | — |
| Reactant | 2-Amino-6-chloro-N-o-tolylbenzamide | HCID 12487367 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 5-Chloro-2-chloromethyl-3-o-tolyl-3H-quinazolin-4-one | HCID 12487373 | 37% |
Reaction Steps
Prepared according to Procedure B with 1j (750 mg, 2.88 mmol) and chloroacetyl chloride (0.69 mL, 8.63 mmol) in acetic acid (15 mL). Purified by chromatography in CH2Cl2, followed by recrystallization from isopropanol to afford 340 mg of a white solid (37%). 1H NMR (CDCl3) δ: 7.69 (d, J=2.1 Hz, 1H); 7.68 (q, J=7.4 Hz, 1H); 7.54 (dd, J=2.2, 7.0 Hz, 1H); 7.35-7.47 (m, 3H); 7.21-7.25 (m, 1H); 4.27 (d, J=12 Hz, 1H); 4.11 (d, J=12 Hz, 1H); 2.18 (s, 3H). MS (ES): m/z 319.0 (M+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08492389B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-ef8cdc8aa52741e7a7b3ea5820a2dd1d |
| Source note | uspto-grants-2013_07 |