3-甲基-2-硫酮-1,3-噻唑啉-4-酮 → 5-[[4-[(4-Acetyl-3-hydroxy-2-propylphenyl)methoxy]phenyl]methylene]-3-methyl-2-thioxo-4-thiazolidinone

HRID 1069120笔记

反应方程式

HRID 1069120 反应方程式
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=2)=[C:6]([CH2:20][CH2:21][CH3:22])[C:5]=1[OH:23])(=[O:3])[CH3:2].C([O-])(=O)C.[Na+].[CH3:29][N:30]1[C:34](=[O:35])[CH2:33][S:32][C:31]1=[S:36]>C(O)(=O)C>[C:1]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][O:11][C:12]2[CH:19]=[CH:18][C:15]([CH:16]=[C:33]3[S:32][C:31](=[S:36])[N:30]([CH3:29])[C:34]3=[O:35])=[CH:14][CH:13]=2)=[C:6]([CH2:20][CH2:21][CH3:22])[C:5]=1[OH:23])(=[O:3])[CH3:2]

参与物

5

反应物 3

HCID 729003-甲基-2-硫酮-1,3-噻唑啉-4-酮HCID 517045醋酸钠HCID 211912774-[(4-Acetyl-3-hydroxy-2-propylphenyl)methoxy]benzaldehyde

产物 1

HCID 867525075-[[4-[(4-Acetyl-3-hydroxy-2-propylphenyl)methoxy]phenyl]methylene]-3-methyl-2-thioxo-4-thiazolidinone

试剂、催化剂与溶剂 1

HCID 176醋酸溶剂

反应条件

温度
100 °C

实验过程

Under a nitrogen atmosphere in a three-neck round bottom flask 4-[(4-acetyl-3-hydroxy-2-propylphenyl)methoxy]benzaldehyde (90.0 mg, 0.29 mmol) was dissolved in acetic acid (1.5 ml) with stirring. To this solution was added sodium acetate (82.8 mg, 1.00 mmol) and N-methylrhodanine (42.5 mg, 0.29 mmol). The reaction mixture was then heated to 100° C. and maintained at this temperature for about two hours at which time the reaction mixture was raised to the reflux temperature and allowed to reflux for about 28 hours. The reaction progress was monitored by thin layer chromatography.

后处理

  1. temperaturemaintained at this temperature for about two hours at which time the reaction mixture
  2. temperaturewas raised to the reflux temperature
  3. temperatureto reflux for about 28 hours

来源与证据

ORD记录
ord-03a655ea75a4460ca91808761dd55d17
来源数据集
uspto-grants-2001_06
专利号
US06251928B1

反应笔记

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