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ChemicalBook CAS DataBase List DIBENZYL DIISOPROPYLPHOSPHORAMIDITE

DIBENZYL DIISOPROPYLPHOSPHORAMIDITE synthesis

5synthesis methods
-

Yield:108549-23-1 75.3%

Reaction Conditions:

with triethylamine in tetrahydrofuran at 0; for 1 h;Inert atmosphere;Cooling with ice;

Steps:

viii (νiii) The synthesis of (i-Pr)2NP(OBn)2 (3-7)
Take compound 3-9, 42g (207.92mmo1) was placed in a 500mL round bottomed flask, was added 300mL of anhydrous tetrahydrofuran, 66mL (455.44mmol, 46g) of anhydrous triethylamine were dissolved with stirring. When the flask was placed in an ice-salt bath until the system temperature was lowered to 0 the right, under nitrogen was added dropwise over anhydrous benzyl alcohol 45mL (416.67mmol, 45g), was added dropwise maintaining temperature of the system is always near 0 , IH complete after the suspension was added dropwise to give a white solid containing the ice bath was removed to room temperature, stirring was continued at room temperature for 3h stirring was stopped to stand 10min, filtered off with suction, washed solid was tetrahydrofuran, the filtrate was collected, rotary evaporated to give tetrahydrofuran was no liquid column liquid chromatography to give an oil 54.0g, a yield of 75.3%.

References:

Nankai University;Xi Zhen;Song Fanbo;Wang Ting;Cui Quanbin;Zhou Kai;Liu Jianbing CN102977145, 2017, B Location in patent:Paragraph 0196; 0197

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