Hydrochloric Acid → 3-Ethoxy-2-methyl-5-[4-(2-pyridyloxy)anilino]-1,8-naphthyridine dihyrochloride trihydrate

HRID 1956454ノート

反応式

HRID 1956454 の反応式
[Cl:1][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.[N:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[O:22][C:23]1[CH:29]=[CH:28][C:26]([NH2:27])=[CH:25][CH:24]=1.[ClH:30]>>[OH2:13].[OH2:22].[OH2:13].[ClH:1].[ClH:30].[CH2:14]([O:13][C:5]1[C:6]([CH3:12])=[N:7][C:8]2[C:3]([CH:4]=1)=[C:2]([NH:27][C:26]1[CH:25]=[CH:24][C:23]([O:22][C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][N:16]=3)=[CH:29][CH:28]=1)[CH:11]=[CH:10][N:9]=2)[CH3:15]

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 131505744-(Pyridin-2-yloxy)anilineHCID 193742665-Chloro-3-ethoxy-2-methyl-1,8-naphthyridine

生成物 1

HCID 675930793-Ethoxy-2-methyl-5-[4-(2-pyridyloxy)anilino]-1,8-naphthyridine dihyrochloride trihydrate

実験手順

A mixture of 5-chloro-3-ethoxy-2-methyl-1,8-naphthyridine (2.0 g) and 4-(2-pyridyloxy)aniline (1.67 g) in IMS (50 ml) was boiled under reflux for 3 hours and then allowed to stand at ambient temperature overnight. The mixture was evaporated under reduced pressure and the residue recrystallised from IMS to give a solid which was dissolved in hot IMS and then cooled in an ice bath while hydrogen chloride gas was bubbled through. The mixture was evaporated to dryness and the residue was recrystallised from IMS to give 3-ethoxy-2-methyl-5-[4-(2-pyridyloxy)anilino]-1,8-naphthyridine dihyrochloride trihydrate, m.p. 244°-247° C. Borderline active (1/1) at 30 mg/kg.

後処理

  1. temperatureunder reflux for 3 hours
  2. customThe mixture was evaporated under reduced pressure
  3. customthe residue recrystallised from IMS
  4. customto give a solid which
  5. customwas bubbled through
  6. customThe mixture was evaporated to dryness
  7. customthe residue was recrystallised from IMS

出典と根拠

ORDレコード
ord-2a6aab8e9ce94a38955b36f526d554db
出典データセット
uspto-grants-1998_07
特許番号
US05780482

反応ノート

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