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Sodium hydride → tert-Butyl{1-[2-(6,7-dimethoxy-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6,7-Dimethoxyquinoxalin-2-ol | HCID 11333210 | — |
| 反応物 | 2-(4-((Tert-butoxycarbonyl)amino)piperidin-1-yl)ethyl methanesulfonate | HCID 56834478 | — |
| 反応物 | tert-butyl {1-[2-(7-methoxy-2-oxoquinolin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate | HCID 59371209 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | tert-Butyl{1-[2-(6,7-dimethoxy-2-oxoquinoxalin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate | HCID 86642646 | 28% |
反応手順
6,7-Dimethoxyquinoxalin-2(1H)-one (Intermediate 158, 540 mg, 2.60 mmol) was deprotonated with sodium hydride (60% in oil, 2.90 mmol) and alkylated with 2-{4-[(tert-butoxycarbonyl)amino]piperidin-1-yl}ethyl methanesulfonate (Intermediate 6) (3.9 mmol) as described for Intermediate 2. Chromatography on silica gel with 20-50% acetone in hexanes gave 310 mg (28%) of the product as an off-white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07875715B2 |
| 出典データセット | uspto-grants-2011_01 |
| ORD ID | ord-85b3b9c7f3904f67ae5d82f452be8629 |
| 出典メモ | uspto-grants-2011_01 |