化工社化工社 化学情報印刷レポート · 研究参考用
Ethanol → Tert-butyl 5-(6-hydroxynaphthalen-2-yl)-2,2-dimethyl-1,3-dioxan-5-ylcarbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanol | HCID 702 | — |
| 反応物 | tert-Butyl (5-(6-(benzyloxy)naphthalen-2-yl)-2,2-dimethyl-1,3-dioxan-5-yl)carbamate | HCID 67424008 | — |
| 触媒 | Palladium hydroxide | HCID 9942167 | — |
| 生成物 | Tert-butyl 5-(6-hydroxynaphthalen-2-yl)-2,2-dimethyl-1,3-dioxan-5-ylcarbamate | HCID 44228963 | 95.3% |
反応手順
[5-(6-Benzyloxy-naphthalen-2-yl)-2,2-dimethyl-1,3-dioxinan-5-yl]-carbamic acid tert-butyl ester (1.19 g, 0.00257 mol) and 20% Pd(OH)2 on carbon (20:80, palladium hydroxide:carbon black, 0.243 g; Aldrich) was suspended in ethanol (200 mL, 3 mol; Fisher), purged with N2 then stirred under H2 (balloon) at r.t. overnight. LCMS showed partial conversion. The mixture was transferred to a pressure vessel and continuously stirred under 50 psi of H2 for one day. The mixture was filtered, evaporated and dried in high vacuum to give a solid product (0.914 g, yield 95.3%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08269043B2 |
| 出典データセット | uspto-grants-2012_09 |
| ORD ID | ord-bbc12533d88841dba0099f2dfb6d833d |
| 出典メモ | uspto-grants-2012_09 |