o-Vanillin → HCID 5111379, 화합물

HRID 1367649노트

반응식

HRID 1367649 반응식
[CH3:1][C:2]1[N:11]([C:12]2[CH:13]=[C:14]([CH3:18])[CH:15]=[CH:16][CH:17]=2)[C:10](=[O:19])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[OH:20][C:21]1[C:28]([O:29][CH3:30])=[CH:27][CH:26]=[CH:25][C:22]=1[CH:23]=O.CC([O-])=O.[Na+]>CC(O)=O>[OH:20][C:21]1[C:28]([O:29][CH3:30])=[CH:27][CH:26]=[CH:25][C:22]=1[CH:23]=[CH:1][C:2]1[N:11]([C:12]2[CH:13]=[C:14]([CH3:18])[CH:15]=[CH:16][CH:17]=2)[C:10](=[O:19])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1

참가 물질

5

반응물 3

HCID 8991o-VanillinHCID 631354(3H)-Quinazolinone, 2-methyl-3-(m-tolyl)-HCID 517045Sodium Acetate

생성물 1

HCID 5111379HCID 5111379, 화합물수율 96.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

In a 50 mL round-bottom flask a mixture of 50 (0.5 g, 002 mol), 2-hydroxy-3 methoxybenzaldehyde (0.4 g, 0.0025 mol) and NaOAc (0.233 g, 0.002 mol) in AcOH was heated under reflux for 10 hours. After cooling the precipitate formed was filtered off, washed with water, dried and recrystallized from acetic acid to yield 51 (0.74 g, 85%). M. Wt. 384. LCMS [M+H]+=385.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 10 hours
  3. temperatureAfter cooling the precipitate
  4. customformed
  5. filtrationwas filtered off
  6. washwashed with water
  7. customdried
  8. customrecrystallized from acetic acid

출처 및 근거

ORD 기록
ord-803615aad5d345e5bb3235257c5694c8
출처 데이터셋
uspto-grants-2011_02
특허 번호
US07893260B2

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