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2-Hydrazinopyridine → HCID 14986969, 화합물

HRID 727782
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HRID 727782 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[C:9](=O)[CH:8]([CH2:14][C:15]([OH:17])=O)[CH2:7][CH2:6]2.[NH:18]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=1)[NH2:19]>C(O)C>[CH3:1][O:2][C:3]1[CH:12]=[CH:11][C:10]2[C:9]3[CH:8]([CH2:14][C:15](=[O:17])[N:18]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=4)[N:19]=3)[CH2:7][CH2:6][C:5]=2[CH:4]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 786452-HydrazinopyridineHCID 13574088(6-Methoxy-1-oxo-1,2,3,4-tetrahydronaphthalen-2-yl)acetic acid

생성물 1

HCID 14986969HCID 14986969, 화합물수율 81.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 20 g of 6-methoxy-1-oxo-1,2,3,4-tetrahydronaphthalene-2-acetic acid, 10.9 g of 2-hydrazinopyridine and 150 ml of ethanol is heated under reflux for 2 hours. The resulting crystals are collected, whereto 50 ml of acetic acid is added. The mixture is heated under reflux for 30 minutes. Acetic acid is distilled off under reduced pressure, and water is added to the residue. The resultant crystals are collected and recrystallized from chloroform - ethanol to give 21.5 g of 8-methoxy-2-(2-pyridyl)-4,4a,5,6-tetrahydrobenzo[h]cinnolin-3(2H)-one as white crystals, m.p. 194°-196° C.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. customThe resulting crystals are collected
  4. additionwhereto 50 ml of acetic acid is added
  5. temperatureThe mixture is heated
  6. temperatureunder reflux for 30 minutes
  7. distillationAcetic acid is distilled off under reduced pressure, and water
  8. additionis added to the residue
  9. customThe resultant crystals are collected
  10. customrecrystallized from chloroform - ethanol

출처 및 근거

ORD 기록
ord-3cc91d8db86e437e969845aa1f00c4d0
출처 데이터셋
uspto-grants-1991_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05045541

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