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Potassium Carbonate → HCID 12235832, 화합물

HRID 2163500
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HRID 2163500 반응식
[Cl-].[NH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N+:4]=1[CH2:9][O:10][C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=1Br.C(=O)([O-])[O-].[K+].[K+]>C(O)CC.O>[CH:15]1[C:16]2[N:2]=[C:3]3[CH:8]=[CH:7][CH:6]=[CH:5][N:4]3[CH2:9][O:10][C:11]=2[CH:12]=[CH:13][CH:14]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 22752766HCID 22752766, 화합물

생성물 1

HCID 12235832HCID 12235832, 화합물수율 60.3%

시약·촉매·용매 2

HCID 962Water용매HCID 10311-Propanol용매

실험 절차

A mixture of 9.5 g of 2-amino-1-[(o-bromophenoxy)methyl]pyridinium chloride, 8.3 g of potassium carbonate, 0.4 g of copper-bronze in 150 ml of n-propanol and 25 ml of water under N2, is heated under reflux for 12 hours while stirring. The mixture is filtered hot and the deep yellow filtrate is concentrated to dryness. The residue is dissolved in 400 ml of ether, the ether solution is washed, dried and the solvent removed to give about 6.4 g of the crude yellow product. This is recrystallized from cyclohexane to give about 3.6 g of the title product, mp about 125°-127°.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 12 hours
  3. filtrationThe mixture is filtered hot
  4. concentrationthe deep yellow filtrate is concentrated to dryness
  5. dissolutionThe residue is dissolved in 400 ml of ether
  6. washthe ether solution is washed
  7. customdried
  8. customthe solvent removed
  9. customto give about 6.4 g of the crude yellow product
  10. customThis is recrystallized from cyclohexane

출처 및 근거

ORD 기록
ord-af0fb47cc9344db290e9a568b627eac7
출처 데이터셋
uspto-grants-1979_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04134975

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