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

HRID 1956454노트

반응식

HRID 1956454 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2a6aab8e9ce94a38955b36f526d554db
출처 데이터셋
uspto-grants-1998_07
특허 번호
US05780482

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