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Hexane → Tert-butyl 6-[(cyclopropylmethoxy)methyl]-6-hydroxy-1,4-oxazepane-4-carboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | Tert-butyl 6-(hydroxymethyl)-1,4-oxazepane-4-carboxylate | HCID 57732267 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Tert-butyl 6-[(cyclopropylmethoxy)methyl]-6-hydroxy-1,4-oxazepane-4-carboxylate | HCID 68531565 | 96% |
反応手順
70-75% m-Chlorobenzenecarboperoxoic acid (145 g, 0.59 mol, 1.2 eq) was added in portions to a stirred solution of tert-butyl 6-(hydroxymethyl)-1,4-oxazepane-4-carboxylate (Preparation 79, 107 g, 0.5 mol, 1 eq) in DCM (1.0 L) that caused heating of the mixture. The reaction mixture was stirred for 24 h at room temperature, then diluted with hexane (500 mL) and filtered. The separated precipitate was washed on a filter with DCM/hexane mixture, and the combined filtrate was washed with aqueous potassium carbonate, dried over sodium sulfate, and evaporated. The residue was vacuum-dried to give title compound (117 g, 0.51 mol, 96%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08357711B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-0ae1292efb73405c9c2a676a5695ae53 |
| 出典メモ | uspto-grants-2013_01 |