2-甲基-2-丁烯 → HCID 178524893，化合物

HRID 43459

反应方程式

HRID 43459 反应方程式
[OH2:1].O.P([O-])(O)(O)=O.[Na+].CC(=CC)C.Cl([O-])=O.[Na+].[F:18][C:19]([F:28])([F:27])[C:20]1[N:21]=[C:22]([CH:25]=[O:26])[NH:23][CH:24]=1>C(O)(C)(C)C>[F:28][C:19]([F:18])([F:27])[C:20]1[N:21]=[C:22]([C:25]([OH:1])=[O:26])[NH:23][CH:24]=1

参与物

6

反应物 4

HCID 105532-甲基-2-丁烯HCID 23668197亚氯酸钠HCID 23673460二水合磷酸二氢钠HCID 178519985HCID 178519985，化合物

产物 1

HCID 178524893HCID 178524893，化合物收率 98%

试剂、催化剂与溶剂 1

HCID 6386叔丁醇溶剂

实验过程

Sodium dihydrogenphosphate dihydrate (720 mg, 4.62 mmol), 2-methyl-2-butene (1.2 ml, 11.4 mmol) and sodium chlorite (420 mg, 4.64 mmol) were added under ice-cooling to a solution of 4-(trifluoromethyl)-1H-imidazole-2-carbaldehyde obtained in Example (33b) (375 mg, 2.29 mmol) in t-butyl alcohol (12 ml)/distilled water (5 ml), followed by stirring for 1.5 hours. The reaction solution was concentrated under reduced pressure, and then the residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water) to obtain 0.402 g of the title compound as a white solid (98%).

后处理

  1. distillation)/distilled water (5 ml)
  2. concentrationThe reaction solution was concentrated under reduced pressure
  3. distillationthe residue was purified by reverse phase silica gel column chromatography (elution solvent: distilled water)

来源与证据

ORD记录
ord-dfb5dbc140d94e42ae20fad4d81cbb8b
来源数据集
uspto-grants-2013_09
专利号
US08536197B2

关联笔记

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