化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → HCID 68862086、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Ethyl orthoformate | HCID 31214 | — |
| 反応物 | Propanediol | HCID 134919 | — |
| 反応物 | 2,6-Dibromobenzaldehyde | HCID 12648641 | — |
| 触媒 | Zirconium chloride (ZrCl4), (T-4)- | HCID 9856075 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | HCID 68862086 | HCID 68862086 | 98% |
反応手順
2,6-Dibromobenzaldehyde (49) (10.0 g, 37.9 mmol) was dissolved in 160 ml dry CH2Cl2. Propanediol (6.4 ml, 88.5 ml), triethylorthoformate (6.83 ml, 41 mmol) and anhydrous ZrCl4 (1.0 g) were added at ambient temperature and stirred overnight. Then NaOH (50 ml of a 10% solution) was added and stirred for an additional hour. The organic phase was separated, the aqueous phase was extracted with Et2O (2×40 ml). The combined organic phases were washed with water (3×60 ml), dried over MgSO4 and the volatiles were removed in vacuo to afford 12 g (98%) 2-(2,6-Dibromophenyl)-1,3-dioxane (acetal) as a slightly yellow solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08969624B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-39a49ebe1c9f419c8d447ac9182f1073 |
| 出典メモ | uspto-grants-2015_03 |