3,4,5-Trimethoxybenzaldehyde → 2-Propenoic acid, 2-azido-3-(3,4,5-trimethoxyphenyl)-, methyl ester

HRID 720326

반응식

HRID 720326 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12])[CH:6]=O.[N:15]([CH2:18][C:19]([O:21][CH3:22])=[O:20])=[N+:16]=[N-:17].[Na]>CO>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:6]=[C:18]([N:15]=[N+:16]=[N-:17])[C:19]([O:21][CH3:22])=[O:20])[CH:8]=[C:9]([O:13][CH3:14])[C:10]=1[O:11][CH3:12]

참가 물질

5

실험 절차

3,4,5-Trimethoxybenzaldehyde (992 mg) and methyl azidoacetate (2.91 g) were dissolved in dry methanol (2 mL), and a dry methanol solution (10 mL) of sodium (582 mg) was added dropwise to the solution at 0° C. over 2 hours under an argon atmosphere. After stirring the reaction mixture for 30 minutes as it is, it was concentrated under reduced pressure, and water was added to the residue to collect crystals deposited by filtration. The crystals were washed with water and dried to obtain the title compound.

후처리

  1. concentrationit was concentrated under reduced pressure, and water
  2. additionwas added to the residue
  3. customto collect crystals
  4. filtrationdeposited by filtration
  5. washThe crystals were washed with water
  6. customdried

출처 및 근거

ORD 기록
ord-2beae094de244f5d962a633e8def4503
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07135473B2

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