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Water → (+/-)-1-(3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydro-2-naphthalenyl)-ethanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Tonalide | HCID 89440 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | (+/-)-1-(3,5,5,6,8,8-Hexamethyl-5,6,7,8-tetrahydro-2-naphthalenyl)-ethanol | HCID 89600820 | 101.1% |
反応手順
A solution of (±)-1-(3,5,5,6,8,8-hexamethyl-5,6,7,8-tetrahydro-2-naphthalenyl)-1-ethanone (10.00 g, 38.7 mmol) in ether (65 ml) was added dropwise during 1 h to a suspension of LiAlH4 (1.48 g, 39.0 mmol) in ether (70 ml) at 0° C. The reaction mixture was left warming up to room temperature and then heated to reflux for 1 day. After cooling to 0° C. more LiAlH4 (0.76 g, 19.5 mmol) was added. After refluxing for another 3 days, the mixture was cooled to 0° C. and water was added dropwise. Extraction of the organic phase with water, drying over Na2SO4 and concentrating gave 10.19 g (99%) of the product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09334464B2 |
| 出典データセット | uspto-grants-2016_05 |
| ORD ID | ord-218c1398bdb54ffc899dc48949dade02 |
| 出典メモ | uspto-grants-2016_05 |