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Dichloromethane → 2-Hydroxy-7,8-dihydro-5(6H)-quinolinone

HRID 875301
ノート
印刷プレビュー

反応式

HRID 875301 の反応式
[NH2:1][C:2]1[CH2:7][CH2:6][CH2:5][C:4](=[O:8])[CH:3]=1.[C:9](OC)(=[O:12])[CH2:10][CH3:11].ClCCl>CO>[NH:1]1[C:2]2[CH2:7][CH2:6][CH2:5][C:4](=[O:8])[C:3]=2[CH:11]=[CH:10][C:9]1=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 11124Methyl propionateHCID 788923-Aminocyclohex-2-en-1-one

生成物 1

HCID 2674502-Hydroxy-7,8-dihydro-5(6H)-quinolinone

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

With stirring, 113.79 g (1.02 mol) of 3-aminocyclohex-2-en-1-one and 114.37 ml (1.19 mol) of methyl propionate were heated at 105° C. for 1 hour. The dark homogeneous solution formed was then slowly heated further to 170° C. After 20 min (temperature: 135° C.), a viscous material formed, and there was a marked evolution of gas. After a further 15 min (temperature: 160° C.), the reaction material became even more viscous while the evolution of gas subsided. After a total of 42 min, a temperature of 170° C. had been reached. After a further 13 min at this temperature, the reaction material was cooled to room temperature. 200 ml of dichloromethane were then added, the mixture was heated briefly and placed into an ultrasonic bath and the crystalline residue formed was filtered off. This procedure was repeated once more with a further 200 ml of dichloromethane. The crystalline residues obtained in this manner were combined, taken up in 1.6 liters of methanol and then heated with stirring until the solid had dissolved completely. This solution was then slowly cooled to room temperature and then stored in a fridge at about 4° C. for 2 days. The crystalline precipitate was filtered off and dried under reduced pressure. This gave 47.65 g (0.29 mol, 29% of theory) of the target product.

後処理

  1. customThe dark homogeneous solution formed
  2. customslowly heated further to 170° C
  3. customa viscous material formed
  4. waitAfter a further 15 min (temperature: 160° C.)
  5. customAfter a total of 42 min
  6. customa temperature of 170° C.
  7. waitAfter a further 13 min at this temperature
  8. temperaturethe mixture was heated briefly
  9. customplaced into an ultrasonic bath
  10. customthe crystalline residue formed
  11. filtrationwas filtered off
  12. customThe crystalline residues obtained in this manner
  13. temperatureheated
  14. stirringwith stirring until the solid
  15. dissolutionhad dissolved completely
  16. temperatureThis solution was then slowly cooled to room temperature
  17. waitstored in a fridge at about 4° C. for 2 days
  18. filtrationThe crystalline precipitate was filtered off
  19. customdried under reduced pressure

出典と根拠

ORDレコード
ord-b897ea16a9ba442aa7c582386b748d27
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08981104B2

反応ノート

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