乙氧基甲叉丙二酸二乙酯 → HCID 178418871，化合物

HRID 7413

反应方程式

HRID 7413 反应方程式
[OH-].[Na+].[CH3:3][S:4][C:5]([NH2:7])=[NH:6].OS(O)(=O)=O.C([O:15][CH:16]=[C:17]([C:23](OCC)=O)[C:18]([O:20][CH2:21][CH3:22])=[O:19])C>C(O)C>[CH3:3][S:4][C:5]1[N:7]=[C:16]([OH:15])[C:17]([C:18]([O:20][CH2:21][CH3:22])=[O:19])=[CH:23][N:6]=1

参与物

5

反应物 3

HCID 6871乙氧基甲叉丙二酸二乙酯HCID 14798二甲基对苯二胺二盐酸HCID 75270S-甲基异硫脲硫酸盐

产物 1

HCID 178418871HCID 178418871，化合物收率 61%

试剂、催化剂与溶剂 1

HCID 702乙醇溶剂

实验过程

To a 4N sodium hydroxide solution (200 mL) was added S-methylisothioureasulfate (55.6 g, 0.2 mol), and after stirring for 30 min, at room temperature a solution of diethyl ethoxymethylenemalonate (80.8 mL, 0.35 mol) in ethanol (100 mL) was dropwise added slowly over 1 h. After stirring for 18 h, the precipitated crystals were collected by filtration, washed several times with cold ethanol and the obtained crystals were added to 1N hydrochloric acid (300 mL). The mixture was stirred for 30 min and the precipitated crystals were collected by filtration, washed several times with cold water and dried with heating under vacuum to give the title compound (26 g, 61%) as crystals.

后处理

  1. additionwas dropwise added slowly over 1 h
  2. filtrationthe precipitated crystals were collected by filtration
  3. washwashed several times with cold ethanol
  4. additionthe obtained crystals were added to 1N hydrochloric acid (300 mL)
  5. stirringThe mixture was stirred for 30 min
  6. filtrationthe precipitated crystals were collected by filtration
  7. washwashed several times with cold water
  8. customdried
  9. temperaturewith heating under vacuum

来源与证据

ORD记录
ord-347b46abced84de9bf8ce6a178260fd5
来源数据集
uspto-grants-2006_08
专利号
US07087597B1

关联笔记

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