ChemicalBook CAS DataBase List Midazolam

Midazolam synthesis

8synthesis methods

Product Name:Midazolam
CAS Number:59467-70-8
Molecular formula:C18H13ClFN3
Molecular Weight:325.77

8-CHLORO-3A,4-DIHYDRO-6-(2-FLUOROPHENYL)-1-METHYL-3H-IMIDAZO[1,5-A][1,4]BENZO-DIAZEPINE

59467-69-5
48 suppliers
$500.50/5MG

59467-70-8
2 suppliers
$16.00/1 mg

Yield:59467-70-8 87%

Reaction Conditions:

with enzyme-containing bacterial cell from Arthrobacter sp. in aq. phosphate buffer; pH=6 at 25; for 15 h;Enzymatic reaction;pH-value;Temperature;

Steps:

10
General procedure: Add Intermediate II to a buffer solution enzyme-containing bacterial cell. The enzyme-containing bacterial cell is the obtained enzyme-containing bacterial cell of Arthrobacter sp. culture. Table 2 shows the stirring speed, reaction time, reaction temperature and buffer solution pH value of bio-catalytic dehydrogenation. High Performance Liquid Chromatography, abbrev. HPLC, track conversion rate. Obtain reaction solution containing Product III. After completing the reaction, use toluene to extract reaction solution. Extract for 3 times. For each time of extraction, the volumetric ratio of toluene and the reaction solution is 1:1. Combine/merge toluene phase. Concentrate toluene phase. Obtain crude product of Product III. Recrystallize crude product to give Product III. Use hydrogen spectrum and carbon spectrum for Product III testing, confirmation of Product III's structure, and calculation of content and molar yield. Dry cell weight of Intermediate II and enzyme-containing bacterial cell by weight ratio is 1:1-50. In Examples 10-18, the weight ratios, respectively, are 1:1,1:5,1:6,1:9,1:10,1:20,1:30,1:40 and 1:50. Stirring speed, reaction time, reaction temperature, buffer solution pH value, content and molar yield are shown in Table 2. In the present example, the buffer solution used is phosphate buffer solution comprising ethanol with volume fraction of 1%-5%. Per liter of buffer solution, it comprises of 5-20g of yeast and 10-30g of agar.

References:

Zhejiang Jiuzhou Pharmaceutical Co., Ltd.;Li, Hong;Pan, Ziguo;Yue, Changlin;Zhang, Jintao;Jia, Yinghua CN103804384, 2016, B Location in patent:Paragraph 0057; 0058; 0059

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