2-甲硫基-4-氯嘧啶 → 4-氟-2-(甲硫基)嘧啶

HRID 9760

反应方程式

HRID 9760 反应方程式
Cl[C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH3:9])[N:3]=1.[F-:10].[K+]>COCCOCCOCCOCCOC.C1OCCOCCOCCOCCOCCOC1>[F:10][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([S:8][CH3:9])[N:3]=1

参与物

5

反应物 2

HCID 971132-甲硫基-4-氯嘧啶HCID 522689氟化钾

产物 1

HCID 102612444-氟-2-(甲硫基)嘧啶收率 63.1%

试剂、催化剂与溶剂 2

HCID 2855718-冠醚-6催化剂HCID 8925四乙二醇二甲醚溶剂

反应条件

温度
150 °C

实验过程

To a solution of 35.7 g (0.22 mol) of 4-chloro-2-methylthiopyrimidine (Aldrich Chemical Co., Milwaukee, Wis., USA) in 135 mL of tetraglyme was added 18-crown-6 (1.33 g) and potassium fluoride (Anhydrous, Aldrich Chemical Co., Milwaukee, Wis., USA, 80 g). The mixture was heated at 150° C.with stirring for 16 hours. The mixture was then cooled and distilled under reduced pressure to give 20 g (62%) of 4-fluoro-2-methylthiopyrimidine as a liquid.

后处理

  1. temperatureThe mixture was then cooled
  2. distillationdistilled under reduced pressure

来源与证据

ORD记录
ord-d02271841a334ff1815f17c48731c924
来源数据集
uspto-grants-2006_08
专利号
US07091347B2

关联笔记

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