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Morpholine → 4-(7-Bromo-2-chloroquinazolin-4-yl)morpholine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Morpholine | HCID 8083 | — |
| 反応物 | 7-Bromo-2,4-dichloroquinazoline | HCID 34176248 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-(7-Bromo-2-chloroquinazolin-4-yl)morpholine | HCID 86665758 | 84% |
反応手順
To an ice cold solution of 7-bromo-2,4-dichloro-quinazoline (7 g, 0.0255 mol) in DCM (150 mL), morpholine (4.43 mL, 0.0509 mol) was slowly added and the reaction was continued at 0° C. for 30 min. The solvent was evaporated to dryness to get the crude compound. The crude product was purified, using column chromatography (60-120 silica gel, 30% ethyl acetate in hexane) to get the title compound (7 g, 84%). 1H NMR (300 MHz, CDCl3): δ 8.17 (d, J=7.5 Hz, 1H), 8.04 (d, J=7.5 Hz, 1H), 7.63 (d, J=8.1 Hz, 1H), 3.72-3.74 (m, 8H): LC-MS (ESI): Calculated mass: 327.0; Observed mass: 329.8 [M+H]+ (RT: 0.45 min).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09115092B2 |
| 出典データセット | uspto-grants-2015_08 |
| ORD ID | ord-5834a6beff6946038c4f093fd2ef07c2 |
| 出典メモ | uspto-grants-2015_08 |