Reaktion #1257709

Reaktionsgleichung

CDI

Boc-D-Val-OH

3,4-Methylenedioxyphenethylamine HCl

triethylamine

→

crude product

Ausbeute 94.6%

(R)—[1-(2-Benzo[1,3]dioxol-5-yl-ethylcarbamoyl)-2-methyl-propyl]-carbamic acid tert-butyl ester

Ausbeute 94.6%

Lösungsmittel

DCE

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.WAITAfter this period
2. 2
   workup.STIRRINGwas stirred at room temperature for 16 hours
3. 3
   EinengenNext, the reaction mixture was concentrated under vacuum
4. 4
   workup.DISSOLUTIONThe crude material was dissolved in DCM (50 mL)
5. 5
   Sonstigetransferred to a separatory funnel
6. 6
   Waschenwashed with sat. NaHCO3 (aq) (50 mL)
7. 7
   Trocknendried over Na2SO4
8. 8
   Einengenconcentrated down

Vorschrift

Boc-D-Val-OH (282 mg, 1.30 mmol) was dissolved in DCE (5 mL), followed by addition of CDI (253 mg, 1.56 mmol). The reaction solution was stirred for 30 mins to activate the acid. After this period, 3,4-Methylenedioxyphenethylamine HCl (263 mg, 1.30 mmol) and triethylamine (363 μL) were added to the reaction vessel and it was stirred at room temperature for 16 hours. Next, the reaction mixture was concentrated under vacuum. The crude material was dissolved in DCM (50 mL), transferred to a separatory funnel, washed with sat. NaHCO3 (aq) (50 mL), dried over Na2SO4 and concentrated down to yield 447.1 mg (94.6%) of crude product, [1-(2-benzo[1,3]dioxol-5-yl-ethylcarbamoyl)-2-methyl-propyl]-carbamic acid tert-butyl ester, which was taken on crude. [M+H]+ 365.00.

Quelle