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Nitric Acid → HCID 178418737, 화합물

HRID 9347
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HRID 9347 반응식
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([OH:12])=[CH:7][CH:8]=[N:9]2)=[CH:4][CH:3]=1.[N+:13]([O-])([OH:15])=[O:14]>C(O)(=O)CC>[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([C:6]([OH:12])=[C:7]([N+:13]([O-:15])=[O:14])[CH:8]=[N:9]2)=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 944Nitric Acid2회HCID 178418765HCID 178418765, 화합물

생성물 1

HCID 178418737HCID 178418737, 화합물수율 78.1%

시약·촉매·용매 1

HCID 1032Propionic Acid용매2회

실험 절차

A stirred suspension of 7-bromoquinolin-4-ol (162 g, 0.723 mol) in propionic acid (1500 mL) was brought to 110° C. 70% Nitric acid (85 g) was added dropwise over 1 h such that the temperature was maintained between 110–115° C. After half of the nitric acid had been added, stirring became difficult due to the formation of solids and an additional 200 mL of propionic acid was added. Upon complete addition, the reaction was stirred for 1 h at 110° C., cooled to room temperature, and the solid was collected by filtration. The filter cake was washed with ice cold ethanol until the washings were nearly colorless (800 mL), and the product was dried at 60° C. under vacuum to afford 152 g of 7-bromo-3-nitro-quinolin-4-ol as a pale yellow solid.

후처리

  1. customwas brought to 110° C
  2. temperaturewas maintained between 110–115° C
  3. additionUpon complete addition
  4. stirringthe reaction was stirred for 1 h at 110° C.
  5. filtrationthe solid was collected by filtration
  6. washThe filter cake was washed with ice cold ethanol until the washings
  7. customthe product was dried at 60° C. under vacuum

출처 및 근거

ORD 기록
ord-b3f9f78625db481c835ecd681b30b45a
출처 데이터셋
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07091214B2

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