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P-Anisidine → 3-Ethoxy-5-(4-methoxyanilino)-2-methyl-1,8-naphthyridine hydrate

HRID 1956436
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HRID 1956436 반응식
Cl[C:2]1[CH:11]=[CH:10][N:9]=[C:8]2[C:3]=1[CH:4]=[C:5]([O:13][CH2:14][CH3:15])[C:6]([CH3:12])=[N:7]2.[CH3:16][O:17][C:18]1[CH:24]=[CH:23][C:21]([NH2:22])=[CH:20][CH:19]=1.[OH-].[Na+]>O>[OH2:13].[CH2:14]([O:13][C:5]1[C:6]([CH3:12])=[N:7][C:8]2[C:3]([CH:4]=1)=[C:2]([NH:22][C:21]1[CH:23]=[CH:24][C:18]([O:17][CH3:16])=[CH:19][CH:20]=1)[CH:11]=[CH:10][N:9]=2)[CH3:15]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 7732P-AnisidineHCID 14798Sodium HydroxideHCID 193742665-Chloro-3-ethoxy-2-methyl-1,8-naphthyridine

생성물 1

HCID 232092353-Ethoxy-5-(4-methoxyanilino)-2-methyl-1,8-naphthyridine hydrate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

The mixture of 5-chloro-3-ethoxy-2-methyl-1,8-naphthyridine (5.0 g), 4-methoxyaniline (2.77 g) and IMS (40 ml) was boiled under reflux for 2.5 hours. The mixture was cooled and filtered. The solid obtained was dissolved in boiling IMS (50 ml) and 5M sodium hydroxide solution (4.0 ml) was added. The mixture was heated under reflux for 1 hour and then cooled and water (100 ml) was added. The mixture was filtered to give 3-ethoxy-5-(4-methoxyanilino)-2-methyl-1,8-naphthyridine hydrate, m.p. 228°-231° C.

후처리

  1. temperatureunder reflux for 2.5 hours
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. customThe solid obtained
  5. dissolutionwas dissolved
  6. additionwas added
  7. temperatureThe mixture was heated
  8. temperatureunder reflux for 1 hour
  9. temperaturecooled
  10. filtrationThe mixture was filtered

출처 및 근거

ORD 기록
ord-8eabe4fb124348e4bc8c9fd6fcf6d758
출처 데이터셋
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05780482

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