Reaktion #821420

Reaktionsgleichung

product

(1S,2S) 2-Ethyl-1-(2-trimethylsilanylethoxycarbonylamino)cyclopropane-carboxylic acid tert-butyl ester

TBAF

THF

→

title intermediate

(1S,2S) 1-Amino-2-ethylcyclopropanecarboxylic acid tert-butyl ester

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe mixture heated
2. 2
   Temperaturto reflux for 1.5 hours
3. 3
   WaschenThe solution was successively washed with water (2×100 mL), brine (2×100 mL)
4. 4
   Trocknendried (MgSO4)
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated in vacuo

Vorschrift

To the product of Step 3 (3 g, 9 mmol) was added a 1.0M TBAF solution in THF (9.3 mL, 9.3 mmol) and the mixture heated to reflux for 1.5 hours, cooled to room temperature and then diluted with 500 mL of ethyl acetate. The solution was successively washed with water (2×100 mL), brine (2×100 mL), dried (MgSO4), filtered, and concentrated in vacuo to provide the title intermediate.

Quelle