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Methanol → N-methoxycarbonylpiperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | 1-Piperidinecarboxylic acid, ethyl ester | HCID 21399 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-methoxycarbonylpiperidine | HCID 232666 | — |
反応手順
Polymer-bound piperidinecarboxylic acid, ethyl ester resin (0.25 g, 0.283 mmol) was swollen with a solution of MeOH (1 ml) in THF (4 ml) in a QUICKFIT test-tube. After addition of sodium methoxide (0.28 ml, 0.028 mmol, 1M solution in MeOH) the resulting suspension was stirred overnight at reflux. The reaction suspension was cooled down to room temperature and the resin was washed using VACMASTER station with DCM (4×3 ml), MeOH (2×3 ml) and then dried under vacuum. FT-IR (2% w/w KBr disk): C=0 1736 cm−1 (ester); 163 cm−1 (amide).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06486354B1 |
| 出典データセット | uspto-grants-2002_11 |
| ORD ID | ord-4b3d8bc8afbd4dad84dbdd0dff1214b2 |
| 出典メモ | uspto-grants-2002_11 |