ChemicalBook CAS DataBase List 1-BENZHYDRYLAZETIDIN-3-ONE

1-BENZHYDRYLAZETIDIN-3-ONE synthesis

7synthesis methods

Product Name:1-BENZHYDRYLAZETIDIN-3-ONE
CAS Number:40320-60-3
Molecular formula:C16H15NO
Molecular Weight:237.3

18621-17-5
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$5.00/1g

40320-60-3
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$6.00/1g

Yield:40320-60-3 96%

Reaction Conditions:

Stage #1:1-(diphenylmethyl)-3-hydroxyazetidine with oxalyl dichloride;dimethyl sulfoxide in dichloromethane at -78; for 1 h;
Stage #2: with triethylamine in dichloromethane

Steps:

1.a; 2.a Example 2:
a. Add oxalyl chloride (106 g, 0.84 mol) to a solution of dimethyl sulfoxide (65.2 g, 0.84 mol) in dichloromethane (2L).Control the reaction temperature at -78 ,Stir for 0.5 hours,Then, a 0.5 liter solution of compound 1 (100 g, 0.42 mol) in dichloromethane was added dropwise at the same temperature. The reaction solution was continuously stirred at -78 ° C for 1 hour.Triethylamine (422 g, 4.2 mol) was added to the reaction system.TLC (petroleum ether / ethyl acetate volume ratio = 1/1) showed the end of the reaction. The reaction solution was added dropwise to a saturated ammonium chloride (1.5 L) solution, and the organic phase was washed four times with 300 mL, dried over anhydrous sodium sulfate, and concentrated in vacuo to obtain a yellow solid compound 2 (96 g, yield 96%).

References:

Shanghai He Quan Pharmaceutical Co., Ltd.;An Ziqiang;Ren Wenwu;Zhou Qiang;Wang Ruiqi;Yang Fang;Yu Peidong;He Yanping;Liu Yueling;Liu Shengpan;Jiao Jiasheng;Xu Fujun;Zhang Lili;Chen Pei;Yu Lingbo;Ma Rujian CN110551133, 2019, A Location in patent:Paragraph 0006; 0013

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