Hydrochloric Acid → (E)-N-(4-(3-(4-hydroxy-3-methylphenyl)acryloyl)-3-methylphenyl)acetamide

HRID 884663노트

반응식

HRID 884663 반응식
[C:1]([C:4]1[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:13])[CH3:12])=[CH:6][C:5]=1[CH3:14])(=[O:3])[CH3:2].[OH-].[Na+].[OH:17][C:18]1[CH:25]=[CH:24][C:21]([CH:22]=O)=[CH:20][C:19]=1[CH3:26].Cl>CCO.O>[OH:17][C:18]1[CH:25]=[CH:24][C:21](/[CH:22]=[CH:2]/[C:1]([C:4]2[CH:9]=[CH:8][C:7]([NH:10][C:11](=[O:13])[CH3:12])=[CH:6][C:5]=2[CH3:14])=[O:3])=[CH:20][C:19]=1[CH3:26]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 1399014-Hydroxy-3-methylbenzaldehydeHCID 27373814'-Acetamido-2'-methylacetophenone

생성물 1

HCID 59349186(E)-N-(4-(3-(4-hydroxy-3-methylphenyl)acryloyl)-3-methylphenyl)acetamide

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매

실험 절차

To a mixture of N-(4-acetyl-3-methylphenyl)acetamide (1.3 g, 7.0 mmol) and NaOH (1.4 g, 36 mmol) in 25 mL of absolute EtOH was added 4-hydroxy-3-methylbenzaldehyde (1.0 g, 7.3 mmol). The reaction mixture was stirred at room temperature for 18 hr. 5 mL of water was added and the reaction mixture was acidified with concentrated HCl to pH 5-6. The aqueous layer was extracted with two 25 mL portions of EOAc, and the layers were separated. The organic layer was dried with Na2SO4, filtered and concentrated under reduced pressure. The resulting product was submitted to the next step without further purification.

후처리

  1. extractionThe aqueous layer was extracted with two 25 mL portions of EOAc
  2. customthe layers were separated
  3. dry with materialThe organic layer was dried with Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting product was submitted to the next step without further purification

출처 및 근거

ORD 기록
ord-bf73e818b71a49028d1c0b7101c0d143
출처 데이터셋
uspto-grants-2012_08
특허 번호
US08242129B2

반응 노트

불러오는 중…