2,3,4,5-TETRAHYDRO-1H-BENZO[E][1,4]DIAZEPINE synthesis
- Product Name:2,3,4,5-TETRAHYDRO-1H-BENZO[E][1,4]DIAZEPINE
- CAS Number:5946-39-4
- Molecular formula:C9H12N2
- Molecular Weight:148.21
![3,4-DIHYDRO-1H-BENZO[E][1,4]DIAZEPINE-2,5-DIONE](/CAS/GIF/5118-94-5.gif)
5118-94-5
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5946-39-4
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Yield: 98%
Reaction Conditions:
Stage #1:1,4-benzodiazepine-2,5-dione with lithium aluminium tetrahydride in tetrahydrofuranCooling with ice;
Stage #2: with ammonium hydroxide in tetrahydrofuran at 20; for 0.666667 h;Cooling with ice;
Steps:
8 Preparation of compound 44-1:
added to compound 43-1 (1.2 g, 6.81 mmol)30 ml of tetrahydrofuran, lithium aluminum hydride (1.2 g, 30.65 mmol) was added in four portions in an ice bath.Each batch was separated by 15 minutes, the ice bath was removed, and the mixture was stirred overnight.The reaction was complete by TLC, the reaction was stopped and cooled to room temperature.A mixed solution of 10 ml of tetrahydrofuran and 1.5 ml of aqueous ammonia was added dropwise under ice bath, and the ice bath was removed.Stir at room temperature for 40 minutes, filter, wash with a small amount of dichloromethane, concentrate the filtrate and purify by column chromatography (CH2Cl2 / MeOH=20/1-10/1)Obtained 980mg of solid,The yield was 98.00%.
References:
Chinese Academy Of Sciences Shanghai Pharmaceutical Institute;Nan Fajun;Li Jia;Gan Linlin;Wang Lei;Chen Linhai;Gao Anhui;Gao Lixin;Zhou Yubo CN109956930, 2019, A Location in patent:Paragraph 0271-0272; 0274
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1000210-73-0
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5946-39-4
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1086096-22-1
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5946-39-4
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28544-83-4
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5946-39-4
65 suppliers
$25.00/250 mg
1000210-73-0
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5946-39-4
65 suppliers
$25.00/250 mg