참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Cesium carbonate | HCID 10796 | — |
| 반응물 | 2-Chloroquinazoline | HCID 74054 | — |
| 반응물 | 3-Amino-4-chlorophenol | HCID 5070078 | — |
| 생성물 | 2-Chloro-5-(6,7-dimethoxyquinazolin-4-yloxy)aniline | HCID 66876386 | — |
반응 단계
A solution of 3-amino-4-chlorophenol (1.00 g, 7.0 mmol) and cesium carbonate (3.38 g, 10.4 mmol) in DMF (20 mL) were heated at 80 C for 1 hr. The chloroquinazoline (1.61 g, 7.2 mmol) was added and the mixture heated for an additional hour. The mixture was poured into water (300 mL) and extracted with EtOAc twice. The combined extracts were washed with brine, dried with magnesium sulfate, filtered and concentrated. The residue was purified using silica gel chromatography eluting with EtOAc/hexane (30-70%), the main peak collected and triturated with DCM to afford 2-chloro-5-(6,7-dimethoxyquinazolin-4-yloxy)aniline. 1H NMR (300 MHz, DMSO d6) δ 3.96 (s, 6H), 5.55 (s, 2H), 6.45 (t, 1H), 6.76 (d, 1H), 7.25 (d, 1H), 7.36 (s, 1H), 7.50 (s, 1H), 8.55 (s, 1H); LC-MS (ESI) m/z 332 (M+H)+
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08969587B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_03 |
|---|
| ORD ID | ord-f6f03001d97f4108ba6db1cc0b1e2793 |
|---|
| 출처 메모 | uspto-grants-2015_03 |
|---|