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Water → 1-ethyl-4-chloro-7-carboxy-1H-pyrazolo[3,4-b]quinoline

HRID 375876
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반응식

HRID 375876 반응식
[CH2:1]([N:3]1[C:7]([NH:8][C:9]2[C:10](=[CH:14][CH:15]=[C:16]([C:18]([OH:20])=[O:19])[CH:17]=2)[C:11](O)=O)=[CH:6][CH:5]=[N:4]1)[CH3:2].O=P(Cl)(Cl)[Cl:23].O>C(O)(=O)C>[CH2:1]([N:3]1[C:7]2=[N:8][C:9]3[C:10]([C:11]([Cl:23])=[C:6]2[CH:5]=[N:4]1)=[CH:14][CH:15]=[C:16]([C:18]([OH:20])=[O:19])[CH:17]=3)[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24813Phosphorus oxychlorideHCID 21217714N-(1-ethylpyrazol-5-yl)-4-carboxyanthranilic acid

생성물 1

HCID 212177041-ethyl-4-chloro-7-carboxy-1H-pyrazolo[3,4-b]quinoline

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A mixture of N-(1-ethylpyrazol-5-yl)-4-carboxyanthranilic acid (2.5 g) and POCl3 (20 ml) was refluxed overnight. The reaction mixture was poured into water, acidified with acetic acid and the solids which formed were collected by filtration. The solid was taken up in 10% NaOH, washed with ether and then the aqueous layer was acidified with concentrated HCl. The mixture was extracted with ether, the ether layer was dried over MgSO4 filtered and evaporated to afford 1 g of 1-ethyl-4-chloro-7-carboxy-1H-pyrazolo[3,4-b]quinoline, as a yellow powder.

후처리

  1. temperaturewas refluxed overnight
  2. customthe solids which formed
  3. filtrationwere collected by filtration
  4. washwashed with ether
  5. extractionThe mixture was extracted with ether
  6. dry with materialthe ether layer was dried over MgSO4
  7. filtrationfiltered
  8. customevaporated

출처 및 근거

ORD 기록
ord-09e56ce5e41046f7ba9c313ab7040747
출처 데이터셋
uspto-grants-1996_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05488055

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