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2-Hydroxy-6-chloroquinoxaline → 6-Chloro-3,4-dihydroquinoxalin-2(1h)-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Hydroxy-6-chloroquinoxaline | HCID 75507 | — |
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-Chloro-3,4-dihydroquinoxalin-2(1h)-one | HCID 283527 | — |
反応手順
Sodium borohydride (5.10 g) is added to a mixture of 6-chloro-1,2-dihydroquinoxalin-2-one (5.60 g), and ethanol (200 ml). The resultant solution is stirred for 2.5 hr at 20°-25°. The material is partitioned between water and ethyl acetate, the phases are separated, the organic phase is dried over magnesium sulfate and concentrated under reduced pressure to give a solid which is recrystallized from ethyl acetate/hexane to give the title compound, mp 171°-174°; IR (mineral oil) 2953, 2925, 1687, 1517, 1408, 1307 and 1299 cm-1 ; NMR (CDCl3 -MeOD) 6.6-6.8 and 3.95 δ; MS (m/z) 182, 153.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05668282 |
| 出典データセット | uspto-grants-1997_09 |
| ORD ID | ord-f7e7c2d8e1cb4d019ba2b747b8d2818e |
| 出典メモ | uspto-grants-1997_09 |