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

HRID 1956436
ノート
印刷プレビュー

反応式

HRID 1956436 の反応式
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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-8eabe4fb124348e4bc8c9fd6fcf6d758
出典データセット
uspto-grants-1998_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05780482

反応ノート

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