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Tetrahydro-4H-pyran-4-one → tert-butyl N-[1-(oxan-4-yl)piperidin-4-yl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Tetrahydro-4H-pyran-4-one | HCID 121599 | — |
| 反応物 | 4-(N-Boc-amino)piperidine | HCID 723833 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | tert-butyl N-[1-(oxan-4-yl)piperidin-4-yl]carbamate | HCID 45792109 | — |
反応手順
A mixture of tert-butyl piperidin-4-ylcarbamate (45 g) and dihydro-2H-pyran-4(3H)-one (24.74 g) in dichloromethane (1000 mL) was treated with sodium triacetoxyborohydride (61.9 g), stirred at room temperature for 16 hours, washed with 1M sodium hydroxide and dried with anhydrous sodium sulfate, filtered and concentrated. The concentrate was flash column chromatographed on silica gel with 10-20% methanol/dichloromethane.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09315488B2 |
| 出典データセット | uspto-grants-2016_04 |
| ORD ID | ord-bf8836a30afa45a8bb5b0c9ec3f3e699 |
| 出典メモ | uspto-grants-2016_04 |