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ChemicalBook CAS DataBase List 7-Benzyl-4,7-diazaspiro[2.5]octane

7-Benzyl-4,7-diazaspiro[2.5]octane synthesis

4synthesis methods
1222106-43-5 Synthesis
W54667

1222106-43-5
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Yield:1222106-45-7 100%

Reaction Conditions:

with sodium tetrahydroborate;boron trifluoride diethyl etherate in tetrahydrofuran at 0; for 20 h;Reflux;Green chemistry;

Steps:

3 Preparation of a compound of formula I

The compound of formula V (804.9 g, 3.49 mol) was suspended in tetrahydrofuran (3 L), sodium borohydride (1056 g, 27.9 mol) was added, cooled to 0 °C in a cold bath, and boron trifluoride diethyl ether (2970 g) was added dropwise. , 20.94mol), after completion, heated reflux reaction for 20h,The reaction solution was cooled to 0 to 10 °C, and 6N aqueous hydrochloric acid solution (6.4 L) was added dropwise to the reaction system, and the temperature was controlled at 30 °C, and the reaction solution was cooled to about 5 °C with a mass fraction of 50% NaOH. The aqueous solution is adjusted to a pH of 9, dichloromethane (3.0 LX 3) is extracted, and the organic phase is combined. Drying to give a brown oil of 706.0 g, the compound of formula I, The yield is 100%.

References:

CN108863958,2018,A Location in patent:Paragraph 0073; 0083; 0084; 0085