碳酸钾 → 4-(4-羟基哌啶-1-基)苯甲醛

HRID 1761818笔记

反应方程式

HRID 1761818 反应方程式
[OH:1][CH:2]1[CH2:7][CH2:6][NH:5][CH2:4][CH2:3]1.F[C:9]1[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=1.C(=O)([O-])[O-].[K+].[K+]>CS(C)=O>[OH:1][CH:2]1[CH2:7][CH2:6][N:5]([C:9]2[CH:16]=[CH:15][C:12]([CH:13]=[O:14])=[CH:11][CH:10]=2)[CH2:4][CH2:3]1

参与物

5

反应物 3

HCID 11430碳酸钾HCID 68023对氟苯甲醛HCID 793414-羟基哌啶

产物 1

HCID 127174464-(4-羟基哌啶-1-基)苯甲醛

试剂、催化剂与溶剂 1

HCID 679二甲基亚砜溶剂

反应条件

温度
95 °C

实验过程

A 2 liter three necked flask fitted with a mechanical stirrer, theromometer and condenser is charged with 180 g of 4-hydroxypiperidine, 74.4 g of 4-fluorobenzaldehyde, 1 ml of Aliquot 336, 750 ml of dimethylsulfoxide and 82.8 g of anhydrous potassium carbonate. The mixture is heated at 95° C. for three days, then the product mixture is cooled and poured into 3 liters of ice water. The resultant solid precipitate is filtered, washed with water, and vacuum dried. The crude product is recrystallized from toluene, m.p. 115°-118° C.

后处理

  1. temperaturethe product mixture is cooled
  2. filtrationThe resultant solid precipitate is filtered
  3. washwashed with water, and vacuum
  4. customdried
  5. customThe crude product is recrystallized from toluene, m.p. 115°-118° C.

来源与证据

ORD记录
ord-91c3f6a03fca4db388c733c79b718e1f
来源数据集
uspto-grants-1989_05
专利号
US04828758

反应笔记

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