N-Cbz-L-histidine synthesis
- Product Name:N-Cbz-L-histidine
- CAS Number:14997-58-1
- Molecular formula:C14H15N3O4
- Molecular Weight:289.29
35016-67-2
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14997-58-1
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$11.00/1g
Yield:14997-58-1 246 g
Reaction Conditions:
with ammonia in dichloromethane at 15 - 38; for 6 h;
Steps:
1-5
The dichloromethane solution of the above bis-CBZ-L-histidine, Cool down to about 15°C, start to pass ammonia gas, and control the temperature of the system to not exceed 30°C. Until the ammonia is saturated. The temperature is raised to reflux, the internal temperature is controlled at about 38°C, and the reaction is carried out for 6 hours. During this time, a white solid will precipitate in the system. After the reaction is over, filter with suction, and the filter cake is to be post-processed. The filtrate is concentrated to dryness, and 2L of petroleum ether is added to make a slurry for 1 hour. The by-product benzyl carbamate is obtained, 129g is obtained after drying, The HPLC content is 98.5%, and the melting point is 85-87°C. The filter cake is recrystallized with 1L isopropanol and cooled to about 10. Suction filtration, vacuum drying, to obtain 246 g of white powdery solid, The total molar yield of the two steps is 75.4%, and the titration content is 100.2%.
References:
CN112898204,2021,A Location in patent:Paragraph 0047; 0055; 0058-0063; 0067-0071; 0074-0079
13795-24-9
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71-00-1
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14997-58-1
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501-53-1
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14997-58-1
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$11.00/1g
71-00-1
869 suppliers
$7.00/5g
14997-58-1
206 suppliers
$11.00/1g