对羟基苯甲醛 → 4-[2-(1,3-Dioxan-2-yl)ethoxy]benzaldehyde

HRID 783

反应方程式

HRID 783 反应方程式
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.Br[CH2:11][CH2:12][CH:13]1[O:18][CH2:17][CH2:16][CH2:15][O:14]1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>C(OCC)(=O)C.C(#N)C>[O:14]1[CH2:15][CH2:16][CH2:17][O:18][CH:13]1[CH2:12][CH2:11][O:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1

参与物

7

反应物 4

HCID 126对羟基苯甲醛HCID 4875碘化钾HCID 11430碳酸钾HCID 5206562-(2-溴乙基)-1,3-二氧杂环己烷

产物 1

HCID 196934674-[2-(1,3-Dioxan-2-yl)ethoxy]benzaldehyde收率 100.2%

试剂、催化剂与溶剂 2

HCID 6342乙腈溶剂HCID 8857乙酸乙酯溶剂

实验过程

In a 500 ml flask, 120 ml of acetonitrile, 13.8 g of 4-hydroxybenzaldehyde, 21.1 g of 2-(2-bromoethyl)-1,3-dioxane, 1.8 g of potassium iodide, and 35.8 g of potassium carbonate were placed and then, reacted at 80° C. for 5 hrs. Thereafter, 200 ml of ethyl acetate was added to the reaction mixture and washed once with a saturated aqueous potassium carbonate solution, distilled water, and saturated saline. The washed organic phase was dried over anhydrous magnesium sulfate and removed solvent, to give 25.6 g of 4-(2-[1,3]-dioxane-2-yl-ethoxy)benzaldehyde.

后处理

  1. customreacted at 80° C. for 5 hrs
  2. washwashed once with a saturated aqueous potassium carbonate solution
  3. distillationdistilled water, and saturated saline
  4. dry with materialThe washed organic phase was dried over anhydrous magnesium sulfate
  5. customremoved solvent

来源与证据

ORD记录
ord-d6f09b988e0848769dd846f380d71108
来源数据集
uspto-grants-1998_03
专利号
US05723258

关联笔记

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