Reaktion #1726687

Reaktionsgleichung

K2CO3

TFA

3A

tert-Butyl 3-(4-(2-oxa-6-azaspiro[3.3]heptan-6-ylmethyl)phenoxy)azetidine-1-carboxylate

K2CO3

→

3B

Ausbeute 94.6%

6-(4-(Azetidin-3-yloxy)benzyl)-2-oxa-6-azaspiro[3.3]heptane

Ausbeute 94.6%

Lösungsmittel

dichloromethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGthe mixture was stirred for 20 min
2. 2
   Sonstigethe mixture was transferred to a separatory funnel
3. 3
   SonstigeThe layers were separated
4. 4
   SonstigeThe combined organic solutions were dried (phase separator)
5. 5
   Sonstigeevaporated

Vorschrift

3A (0.19 g, 0.52 mmol) was dissolved in dichloromethane (20 mL) and TFA (1.95 mL, 26 mmol) was added. The reaction mixture was stirred at room temperature for two hours. K2CO3 (5 g) was added in portions and the mixture was stirred for 20 min. A saturated solution of K2CO3 (aq) was added and the mixture was transferred to a separatory funnel. The layers were separated and the aqueous layer was further extracted several times with dichloromethane. The combined organic solutions were dried (phase separator) and evaporated. There was obtained 128 mg (94%) of 3B as an oil. 1H NMR (500 MHz, CDCl3): δ 3.34 (s, 4H), 3.45 (s, 2H), 3.80 (m, 2H), 3.92 (m, 2H), 4.72 (s, 4H), 4.98 (m, 1H), 6.69 (d, 2H), 7.13 (d, 2H), MS (APCI+) m/z 261 [M+H]+.

Quelle