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Ammonium Hydroxide → 1-ethyl-4-chloro-7-methoxy-1H-pyrazolo[3,4-b]quinoline

HRID 977130
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반응식

HRID 977130 반응식
[CH2:1]([N:3]1[C:7]([NH:8][C:9]2[C:10](=[CH:14][CH:15]=[C:16]([O:18][CH3:19])[CH:17]=2)[C:11](O)=O)=[CH:6][CH:5]=[N:4]1)[CH3:2].O=P(Cl)(Cl)[Cl:22].[NH4+].[OH-]>>[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:10]([C:11]([Cl:22])=[C:6]2[CH:5]=[N:4]1)=[CH:14][CH:15]=[C:16]([O:18][CH3:19])[CH:17]=3)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 14923Ammonium HydroxideHCID 24813Phosphorus oxychloride2회HCID 19592233N-(1-ethylpyrazol-5-yl)-4-methoxyanthranilic acid

생성물 1

HCID 195922181-ethyl-4-chloro-7-methoxy-1H-pyrazolo[3,4-b]quinoline수율 87%

실험 절차

A mixture of N-(1-ethylpyrazol-5-yl) -4-methoxyanthranilic acid (13.3 g, 0.051 mol) and POCl3 (125 ml) was refluxed for 3 hours, then was allowed to sit overnight. The volume of POCl3 was reduced, then ice/water, followed by NH4OH was added. A precipitate formed which was collected by filtration and dried in a vacuum oven at 50° C. to afford 11.51 g (87%) of 1-ethyl-4-chloro-7-methoxy-1H-pyrazolo[3,4-b]quinoline, m.p. 95°-98° C.

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후처리

  1. temperaturewas refluxed for 3 hours
  2. additionwas added
  3. customA precipitate formed which
  4. filtrationwas collected by filtration
  5. customdried in a vacuum oven at 50° C.

출처 및 근거

ORD 기록
ord-c55f0137e5114da9b079ae3f4067b92b
출처 데이터셋
uspto-grants-1997_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05614530

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