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HRID722854

反应详情

EQUATION

反应方程式

HRID 722854 的结构方程式

REACTANTS

反应物

4
结构：O
HCID962

Water

H2O

结构：[H-].[Na+]
HCID24758

Sodium hydride

HNa

结构：COC(=O)C(C)C(=O)OC
HCID69104

Propanedioic acid, methyl-, dimethyl ester

C6H10O4

结构：C[C@@H](c1ccccc1)N1C[C@@H](CI)CC1=O
HCID10830178

未命名化合物

PRODUCTS

生成物

1
结构：COC(=O)C(C)(C[C@H]1CC(=O)N([C@@H](C)c2ccccc2)C1)C(=O)OC
HCID59094041

未命名化合物

收率 81%

AUXILIARIES

试剂、催化剂与溶剂

1
结构：CS(C)=O
溶剂HCID679

Dimethyl sulfoxide

C2H6OS

2 次

PROCEDURE

实验过程

To dimethyl methylmalonate (1.06 g, 7.29 mmol) in DMSO (7 mL) at room temperature was added NaH (291 mg of a 60% dispersion in oil). After the effervescence had ceased the lactam 85 (2 g, 7.29 mol) in DMSO (5 mL) was added. After 1 hour water was added and the aqueous solution extracted with ether. The combined organic extracts were dried (MgSO4) and concentrated. Flash chromatography (1:1 hexane/acetone) of the residue gave the product as an oil (1.7 g, 81%). MS m/z 348 (M+H, 100%).

WORKUP

后处理

  1. additionwas added
  2. extractionthe aqueous solution extracted with ether
  3. dry with materialThe combined organic extracts were dried (MgSO4)
  4. concentrationconcentrated