3,4-DIHYDRO-2H-1,5-BENZODIOXEPIN-7-AMINE synthesis

Yield:175136-34-2 61%

Reaction Conditions:

with iron;ammonium chloride in ethanol;water for 4 h;Reflux;

Steps:

63.2 Step two:Synthesis of 7-amino-3,4-dihydro-2H-1,5-benzodioxepane
(1.00g, 5.12mmol),Reduced iron powder (1.10g, 19.69mmol),Ammonium chloride (2.20g, 41.12mmol) was added to ethanol (20mLAnd water (20mL),Heat to reflux and stir for 4 hours,TLC (PE:EA=10:1) showed that the reaction was complete.The reaction liquid is filtered while hot,Ethanol washing,concentrate,Add water (20mL),Ethyl acetate extraction,Combine the organic phases,Wash with saturated brine,Dry with anhydrous sodium sulfate,filter,concentrate,Crude silica gel column chromatography (PE:EA=10:15:1) purification,A light brown solid (0.52 g, 61percent yield) was obtained.

References:

Shaoxing Cong Ling Pharmaceutical Technology Co., Ltd.;Sichuan University Huaxi Hospital;East China Normal University;Yang Huaiyu;Jiang Ruotian;Zhang Qiansen CN111548313, 2020, A Location in patent:Paragraph 0322-0328

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