Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Tert-Butylamine | HCID 6385 | — |
| Reactant | HCID 89782153 | HCID 89782153 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 89782161 | HCID 89782161 | — |
Reaction Steps
A mixture of tert-butylamine (1.1 mL, 10.43 mmol) and 8-bromo-2-chloro-3-ethylquinazolin-4(3H)-one (100 mg, 0.348 mmol, 481c) was sealed and set stirring for 3 h at 80° C. The reaction was cooled to RT, diluted with water, and extracted with DCM. The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure giving a pale yellow solid. The material was taken up DCM, adsorbed onto silica, and purified on 4 g SiO2 (eluent: 0-100% EtOAc/hexanes over 20 min, RediSep Gold). The product containing fractions were combined and concentrated under reduced pressure to a colorless residue (52 mg, 46%). m/z (ESI, +ve) 323.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09394297B2 |
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| Source dataset | uspto-grants-2016_07 |
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| ORD ID | ord-08fb9e4731624ce88b0b5d3a3c5eef02 |
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| Source note | uspto-grants-2016_07 |
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