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Sodium hydride → tert-Butyl 4-[2-(6-methoxy-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)propyl]piperazine-1-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 6-methoxy-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 13204952 | — |
| 反応物 | tert-Butyl 4-(3-((methylsulfonyl)oxy)propyl)piperazine-1-carboxylate | HCID 15540662 | — |
| 反応物 | tert-butyl {1-[2-(7-methoxy-2-oxoquinolin-1(2H)-yl)ethyl]piperidin-4-yl}carbamate | HCID 59371209 | — |
| 溶媒 | Isopropanol methylene chloride | HCID 21966342 | — |
| 生成物 | tert-Butyl 4-[2-(6-methoxy-3-oxo-2,3-dihydro-4H-1,4-benzoxazin-4-yl)propyl]piperazine-1-carboxylate | HCID 86642636 | — |
反応手順
6-Methoxy-2H-1,4-benzoxazin-3(4H)-one (Intermediate 48, 440 mg, 2.5 mmol) was deprotonated with sodium hydride (125 mg, 60% in oil, 3.2 mmol) and alkylated with tert-butyl 4-{3-[(methylsulfonyl)oxy]propyl}piperazine-1-carboxylate (Intermediate 120, 2.5 mmol) as described for Intermediate 2. Chromatography on silica gel with dichloromethane/2-propanol (95:5) gave 1.25 g (quantitative) of the product as a yellow oil.
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-d78d77cdd86c445dad62028cb6e55f50 |
| 出典メモ | uspto-grants-2011_01 |