3-(4,5-DIHYDRO-1-METHYL-1H-PYRROL-2-YL)PYRIDINE synthesis
- Product Name:3-(4,5-DIHYDRO-1-METHYL-1H-PYRROL-2-YL)PYRIDINE
- CAS Number:525-74-6
- Molecular formula:C10H12N2
- Molecular Weight:160.22
626-55-1
539 suppliers
$5.00/5 / G
872-50-4
877 suppliers
$10.00/100ML
525-74-6
20 suppliers
$250.00/1 mg
Yield: 81%
Reaction Conditions:
Stage #1:3-Bromopyridine with ethyl bromide;magnesium in tetrahydrofuran at 25 - 30; for 3 h;Inert atmosphere;
Stage #2:1-methyl-pyrrolidin-2-one in tetrahydrofuran at 20 - 25;Inert atmosphere;Temperature;
Steps:
1; 3; 5; 7 Example 1:
Add 2.85g magnesium shavings to a clean three-necked bottle,30ml of anhydrous THF, equipped with magnets, condenser, nitrogen balloon replacement;Add 2.2g of bromoethane initiator in one portion and stir at about 25 ° C at room temperature.Wait for initiation (heating, mixing); after initiation,Start to dropwise add a mixed solution of THF and 3-bromopyridine (mass ratio of THF to 3-bromopyridine is 2: 1, 16g of 3-bromopyridine and 32g of THF),Keep the temperature controlled at about 30 ° C for the reaction; after dripping, continue to incubate for 3 hours,After cooling to about 20 ;The dropwise addition of a mixed solution of N-methylpyrrolidone and THF (7 g of N-methylpyrrolidone and 20 g of THF) was started,The temperature is controlled between 25 ° C. After the dropwise addition, transfer to room temperature and react overnight;The next day, the reaction was quenched by the dropwise addition of 6N (ie: 6mol / L) hydrochloric acid at about 25 ° C.Adjust the pH to between 3 and 4; then add 6N Alkaliliquid to adjust the pH to about 10,Dichloromethane was added for extraction twice; the organic phases were combined, dried, concentrated,Distillation gave 9.15 g of an enamine intermediate as a pale yellow oil. Yield was 81%.
References:
Jinan Wu Tong Biological Technology Co., Ltd.;Gao Ming;Li Xin;Wang Jianan;Wang Yunguang;Li Shanke CN110357853, 2019, A Location in patent:Paragraph 0040; 0049-0050; 0054-0055; 0057-0058; 0060-0061
125630-28-6
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$100.00/100mg
525-74-6
20 suppliers
$250.00/1 mg
54-11-5
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$15.60/250mg
525-74-6
20 suppliers
$250.00/1 mg
494-97-3
71 suppliers
$109.00/100mg