BIIB-021 synthesis
- Product Name:BIIB-021
- CAS Number:848695-25-0
- Molecular formula:C14H15ClN6O
- Molecular Weight:318.76
86604-75-3
562 suppliers
$10.00/1g
10310-21-1
535 suppliers
$10.00/5g
848695-25-0
127 suppliers
$39.00/1mg
Yield:848695-25-0 77%
Reaction Conditions:
Stage #1: 2-amino-6-chloropurinewith potassium carbonate in dimethyl sulfoxide at 48; for 0.5 h;
Stage #2: 2-(chloromethyl)-4-methoxy-3,5-dimethylpyridine hydrochloride in dimethyl sulfoxide at 22 - 48; for 12.5 h;
Steps:
1 1. Synthesis of parent drug
Weigh respectively 2-amino-6-chloropurine 10mmol, anhydrous potassium carbonate 12mmol, the amount of 25mL DMSO was added to a 50mL round bottom flask, the oil bath was heated to 48 ° C, stirring reaction 30min;11 mmol of 2-chloromethyl-3,5-dimethylpyridine hydrochloride was weighed and added to the above reaction solution in 3 portions at intervals of 30 minutes.After reacting at 48 °C for 10 h, the temperature was set to 22 °C and stirred for 2 h. After the reaction was completed, the reaction solution was filtered and the filtrate was retained.The volume ratio of water: isopropyl alcohol = 1:1 mixed solution was added to the filtrate, until the solution became turbid to stop dropping, and the solution was placed in a refrigerator to stand still overnight. The filter residue was parent molecule BIIB021. 6-Chloro-9-[(4-methoxy-3,5-dimethyl-2-pyridyl)methyl]-9H-purin-2-amine (BIIB021):Light yellow solid; Yield: 77%;
References:
CN107857763,2018,A Location in patent:Paragraph 0014-0016
86604-75-3
562 suppliers
$10.00/1g
10310-21-1
535 suppliers
$10.00/5g
848695-25-0
127 suppliers
$39.00/1mg