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o-Vanillin → HCID 136400709, 화합물

HRID 1367651
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HRID 1367651 반응식
[CH3:1][C:2]1[N:11]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([Cl:19])[CH:13]=2)[C:10](=[O:20])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH:21][C:22]1[C:29]([O:30][CH3:31])=[CH:28][CH:27]=[CH:26][C:23]=1[CH:24]=O.CC([O-])=O.[Na+]>CC(O)=O>[Cl:19][C:14]1[CH:13]=[C:12]([N:11]2[C:10](=[O:20])[C:9]3[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=3)[N:3]=[C:2]2[CH:1]=[CH:24][C:23]2[CH:26]=[CH:27][CH:28]=[C:29]([O:30][CH3:31])[C:22]=2[OH:21])[CH:17]=[CH:16][C:15]=1[Cl:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 8991o-VanillinHCID 517045Sodium AcetateHCID 5888673-(3,4-dichlorophenyl)-2-methylquinazolin-4-one

생성물 1

HCID 136400709HCID 136400709, 화합물수율 71%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Compound 63 (1 g, 0.028 mol), 2-hydroxy-3 methoxybenzaldehyde (9, 0.4 g, 0.003 mol) and NaOAc (0.233 g, 0.002 mol) in AcOH were heated under reflux for 10 hours. After cooling the precipitate formed was washed with water, filtered off, dried and recrystallized from EtOH to yield 64 (0.55 g, 71%). M. Wt. 439. LCMS [M+H]+=440.

후처리

  1. temperatureunder reflux for 10 hours
  2. temperatureAfter cooling the precipitate
  3. customformed
  4. washwas washed with water
  5. filtrationfiltered off
  6. customdried
  7. customrecrystallized from EtOH

출처 및 근거

ORD 기록
ord-2d31bad3cef14be690c3a95c144dc3d0
출처 데이터셋
uspto-grants-2011_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07893260B2

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