Acetyl chloride → (5-(Benzyloxy)-4-oxo-1,4-dihydropyridin-2-yl)methyl acetate

HRID 385569

반응식

HRID 385569 반응식
[CH2:1]([O:8][C:9]1[C:10](=[O:17])[CH:11]=[C:12]([CH2:15][OH:16])[NH:13][CH:14]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[C:18](Cl)(=[O:20])[CH3:19]>N1C=CC=CC=1>[C:18]([O:16][CH2:15][C:12]1[NH:13][CH:14]=[C:9]([O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)[C:10](=[O:17])[CH:11]=1)(=[O:20])[CH3:19]

참가 물질

4

반응물 2

HCID 6367Acetyl chlorideHCID 28015645-(Benzyloxy)-2-(hydroxymethyl)-1,4-dihydropyridin-4-one

생성물 1

HCID 57815284(5-(Benzyloxy)-4-oxo-1,4-dihydropyridin-2-yl)methyl acetate

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
65 °C

실험 절차

To a solution of 10 g of 5-(benzyloxy)-2-(hydroxymethyl)pyridin-4(1H)-one in 58 mL of pyridine, 4.6 mL of acetyl chloride was added under cooling with ice, and the mixture was stirred at 60 to 70° C. for 3 hours. The solvent was distilled off under reduced pressure, water was added thereto, and the mixture was stirred under cooling with ice. The solid was filtered off, chloroform was added thereto and the resultant was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure. Thereto was added diethyl ether and the solid was filtered off to obtain 9.2 g of (5-(benzyloxy)-4-oxo-1,4-dihydropyridin-2-yl)methyl acetate as a light brown solid.

후처리

  1. temperatureunder cooling with ice
  2. distillationThe solvent was distilled off under reduced pressure, water
  3. additionwas added
  4. stirringthe mixture was stirred
  5. temperatureunder cooling with ice
  6. filtrationThe solid was filtered off
  7. additionchloroform was added
  8. dry with materialthe resultant was dried over anhydrous magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure
  10. additionThereto was added diethyl ether
  11. filtrationthe solid was filtered off

출처 및 근거

ORD 기록
ord-05200f01122c426284034e7a3ea50130
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08367831B2

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