反应详情

The compound of step 3 (395 mg, 1.31 mmol) was dissolved in DCM (5 ml). DMF (29 mg, 0.39 mmol) and oxalyl chloride (3.9 ml of a 2 M solution in DCM) were added at room temperature. The mixture was stirred for 60 min, evaporated to dryness in vacuo, dissolved in dioxane and evaporated again. The residue was dissolved in DCM (2 ml) and the solution was slowly added with stirring to an ice-cooled mixture of 2-amino-indane-2-carboxylic acid methyl ester hydrochloride (5.42 g, 23.8 mmol), EA and an excess of saturated aqueous sodium hydrogencarbonate solution. After 2 h, the organic layer was separated, washed with a saturated sodium chloride solution, dried over sodium sulfate, filtered and evaporated to dryness. 582 mg of the title compound were obtained.

1. customevaporated to dryness in vacuo
2. dissolutiondissolved in dioxane
3. customevaporated again
4. dissolutionThe residue was dissolved in DCM (2 ml)
5. additionthe solution was slowly added
6. stirringwith stirring to an ice-
7. temperaturecooled
8. waitAfter 2 h
9. customthe organic layer was separated
10. washwashed with a saturated sodium chloride solution
11. dry with materialdried over sodium sulfate
12. filtrationfiltered
13. customevaporated to dryness