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HRID440135

反应详情

EQUATION

反应方程式

HRID 440135 的结构方程式

REACTANTS

反应物

3
结构：O=C([O-])[O-].[Na+].[Na+]
HCID10340

Carbonic acid sodium salt (1:2)

CNa2O3

结构：CC(C)(C)NC(=O)[C@@H]1C[C@@H]2CCCC[C@@H]2CN1
HCID454736

(3S,4aS,8aS)-N-tert-Butyldecahydroisoquinoline-3-carboxamide

C14H26N2O

结构：O=C1N[C@@H](Cc2ccccc2)[C@@H](COS(=O)(=O)c2ccc([N+](=O)[O-])cc2)O1
HCID11058277

[(4S,5S)-2-Oxo-4-(phenylmethyl)-5-oxazolidinyl]methyl 4-nitrobenzenesulfonate

C17H16N2O7S

PRODUCTS

生成物

1
结构：CC(C)(C)NC(=O)[C@@H]1C[C@@H]2CCCC[C@@H]2CN1C[C@H]1OC(=O)N[C@H]1Cc1ccccc1.O=[N+]([O-])c1ccc(S(=O)(=O)O)cc1
HCID86749025

未命名化合物

收率 88.4%

AUXILIARIES

试剂、催化剂与溶剂

2
结构：Cl
溶剂HCID313

Hydrochloric Acid

ClH

结构：CC(=O)CC(C)C
溶剂HCID7909

4-Methyl-2-pentanone

C6H12O

2 次

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of 24.69 g of p-nitrobenzenesulphonic acid (4S, 5S)-4-benzyl-2-oxo-oxazolidin-5-ylmethyl ester (Example 12), 15.0 g of N-tert.butyl-decahydro-(4aS,8aS)-isoquinoline-3(S)-carboxamide and 10.0 g of sodium carbonate in 76 ml of 4-methyl-2-pentanone is heated under reflux for 10 hours while stirring. The suspension is cooled to 80° C., diluted with 178 ml of 4-methyl-2-pentanone and 54 ml of 3N hydrochloric acid, cooled to 40° C and filtered. The residue is washed with water and 4-methyl-2-pentanone and dried to give 35.1 g (88%) of (3S, 4aS ,8aS)-2-[(4S,5R)-4-benzyl-2-oxo-oxazolidin-5-ylmethyl]-N-tert.butyl -decahydro-isoquinoline-3-carboxamide p-nitrobenzenesulphonate, [α]D20 =-31.2° (1% in DMF).

WORKUP

后处理

  1. temperatureis heated
  2. temperatureunder reflux for 10 hours
  3. temperaturecooled to 40° C
  4. filtrationfiltered
  5. washThe residue is washed with water and 4-methyl-2-pentanone
  6. customdried