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

HRID 987434

반응식

HRID 987434 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

반응물 3

HCID 68583,4,5-TrimethoxybenzaldehydeHCID 4020482Methyl 2-azidoacetateHCID 5360545Sodium

생성물 1

HCID 43062472-Propenoic acid, 2-azido-3-(3,4,5-trimethoxyphenyl)-, methyl ester

시약·촉매·용매 1

HCID 887Methanol용매2회

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-5a1ac44a49bb4182843c9dc9adb3e443
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06632810B2

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