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HRID392309

反应详情

EQUATION

反应方程式

HRID 392309 的结构方程式

REACTANTS

反应物

3
结构：COC(OC)OC
HCID9005

Trimethoxymethane

C4H10O3

结构：Cc1ccc(S(=O)(=O)O)cc1.O
HCID521998

4-Methylbenzenesulfonic acid hydrate

C7H10O4S

结构：COC(=O)c1nccn([C@@H]2O[C@H](CO)[C@@H](O)[C@H]2O)c1=O
HCID11492964

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)c1nccn([C@@H]2O[C@H](CO)[C@H]3OC(C)(C)O[C@H]32)c1=O
HCID60126642

未命名化合物

收率 865.6%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CC(C)=O
溶剂HCID180

Acetone

C3H6O

PROCEDURE

实验过程

In 5 mL of acetone was suspended 0.50 g of methyl 4-[(2R,3R,4S,5R)-3,4-dihydroxy-5-(hydroxymethyl)tetrahydro-2-furanyl]-3-oxo-3,4-dihydro-2-pyrazinecarboxylate. Then, 1 ml of trimethyl orthoformate and 33 mg of p-toluenesulfonic acid monohydrate were successively added, the mixture thus obtained was heated under reflux for one hour, and the solvent was removed under reduced pressure. By purifying the residue by column chromatography [eluent: ethyl acetate], 0.49 g of methyl 4-[(3aR,4R,6R,6aR)-6-(hydroxymethyl)-2,2-dimethyltetrahydrofuro[3,4-d][1,3]dioxol-4-yl]-3-oxo-3,4-dihydro-2-pyrazinecarboxylate was obtained as a white-colored solid product.

WORKUP

后处理

  1. customthe mixture thus obtained
  2. temperaturewas heated
  3. temperatureunder reflux for one hour
  4. customthe solvent was removed under reduced pressure
  5. customBy purifying the residue by column chromatography [eluent: ethyl acetate]