化工社化工社 化学情報印刷レポート · 研究参考用
Methanol → 5-(tert-Butyl-dimethyl-silanyloxy)-cyclooctanecarbonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanol | HCID 887 | — |
| 反応物 | Tosylmethyl isocyanide | HCID 161915 | — |
| 反応物 | 5-(Tert-butyldimethylsilyloxy)cyclooctanone | HCID 10978090 | — |
| 反応物 | Potassium tert-butoxide | HCID 23665647 | — |
| 溶媒 | 1,2-Dimethoxyethane | HCID 8071 | — |
| 生成物 | 5-(tert-Butyl-dimethyl-silanyloxy)-cyclooctanecarbonitrile | HCID 66656929 | — |
反応手順
Potassium tert-butoxide (30.4 mL, 1 M in tetrahydrofuran, 30.4 mmol) was added drop wise to a stirred and cooled (0° C.) solution of tosylmethyl isocyanide (4.74 g, 24.27 mmol) in dry DME (40 mL). After ten minutes, dry methanol (0.98 mL, 24.28 mmol) was added and followed by a solution of the product of Example 5B (3.11 g, 12.14 mmol) in DME (10 mL). The resulting solution was allowed to warm to room temperature and then heated (45° C.) for thirty minutes. After cooling, the reaction mixture was partitioned with diethyl ether and water. The organic phase was washed with brine, dried (MgSO4), filtered, and evaporated. The residue was purified over silica gel using 2-10% diethyl ether in hexanes to give the title compound as an oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07737137B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-50778fe737ce4361906f6b8f685034de |
| 出典メモ | uspto-grants-2010_06 |