化工社化工社 化学情報印刷レポート · 研究参考用
Water → HCID 58406163、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 1-Pyrrolidinecarbonyl chloride | HCID 70937 | — |
| 反応物 | (11S)-6-amino-11-methyl-10,11-dihydro-8H-[1,4]oxazino[4',3':1,2]imidazo[4,5-c]quinolin-2-ol | HCID 58406167 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 58406163 | HCID 58406163 | 17.9% |
反応手順
A solution of (11S)-6-amino-11-methyl-10,11-dihydro-8H-[1,4]oxazino[4′,3′:1,2]imidazo[4,5-c]quinolin-2-ol (500 mg, 1.85 mmol) dissolved in 15 mL of DMF was treated with cesium carbonate (1.80 g, 5.55 mmol) and pyrrolidinecarbonyl chloride (275 mg, 2.03 mmol). After stirring overnight at ambient temperature, the light brown mixture was poured into 150 mL of H2O and stirred for 30 minutes. The reaction mixture was extracted with CHCl3 (3×75 mL) and the combined extracts were dried over MgSO4, filtered and concentrated under reduced pressure to give a brown solid. Chromatography (SiO2, 0-20% CMA/CHCl3) gave an off-white solid which was crystallized from acetonitrile to give 122 mg of the title compound as an off-white solid, mp 218-219° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08207162B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-68bc82118c8d4fbdaa40c9cdde20e58f |
| 出典メモ | uspto-grants-2012_06 |