异氰酸-4-氯-2-氟苯酯 → 3-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine

HRID 27005

反应方程式

HRID 27005 反应方程式
[C:1]([CH:6]1[CH2:11][S:10][CH2:9][CH2:8][NH:7]1)([O:3][CH2:4][CH3:5])=[O:2].[Cl:12][C:13]1[CH:18]=[CH:17][C:16]([N:19]=[C:20]=[O:21])=[C:15]([F:22])[CH:14]=1>CCCCCC.CCOCC>[C:1]([CH:6]1[CH2:11][S:10][CH2:9][CH2:8][N:7]1[C:20]([NH:19][C:16]1[CH:17]=[CH:18][C:13]([Cl:12])=[CH:14][C:15]=1[F:22])=[O:21])([O:3][CH2:4][CH3:5])=[O:2]

参与物

5

反应物 2

HCID 4558203异氰酸-4-氯-2-氟苯酯HCID 13604869硫代吗啉-3-羧酸乙酯

产物 1

HCID 233433973-Carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine收率 87.7%

试剂、催化剂与溶剂 2

HCID 3283乙醚溶剂HCID 8058正己烷溶剂

实验过程

An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.

后处理

  1. customA heavy oil formed
  2. additionafter the addition
  3. customThe oil crystallized
  4. stirringafter stirring at room temperature for 15 min
  5. filtrationThe precipitate was collected by filtration

来源与证据

ORD记录
ord-95b0801eb1af422b91d722b853fc31cf
来源数据集
uspto-grants-1980_09
专利号
US04220465

关联笔记

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