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Allyl iodide → 5-Allyloxy-3,8-dimethylcarbostyril

HRID 1900808
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인쇄 미리보기

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HRID 1900808 반응식
[OH:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[C:5]([CH3:14])[C:6](=[O:13])[NH:7]2.[CH2:15](I)[CH:16]=[CH2:17].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:17]([O:1][C:2]1[CH:11]=[CH:10][C:9]([CH3:12])=[C:8]2[C:3]=1[CH:4]=[C:5]([CH3:14])[C:6](=[O:13])[NH:7]2)[CH:16]=[CH2:15]
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참가 물질

5

반응물 3

HCID 11166Allyl iodideHCID 11430Potassium CarbonateHCID 233696243,8-Dimethyl-5-hydroxycarbostyril

생성물 1

HCID 233695515-Allyloxy-3,8-dimethylcarbostyril수율 89.2%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
70 °C

실험 절차

5-Hydroxy-3,8-dimethylcarbostyril (4 g, 21.16 mmol) and allyl iodide (3.73 g, 22.2 mmol) were dissolved in dimethylformamide (44 ml), to which potassium carbonate (6.1 g, 44.2 mmol) was added, and stirred for 2 hours in a bath at 70° C. The solvent was distilled off, and the residue was dissolved in chloroform, and washed with water. After drying and condensing, the resultant residue was purified by silica gel chromatography (chloroform), and was subjected to recrystallization (chloroform-n-hexane) to obtain 4.32 g of the title compound as pale yellow prisms (89.2%).

후처리

  1. additionwas added
  2. distillationThe solvent was distilled off
  3. dissolutionthe residue was dissolved in chloroform
  4. washwashed with water
  5. customAfter drying
  6. customcondensing
  7. customthe resultant residue was purified by silica gel chromatography (chloroform)
  8. customwas subjected to recrystallization (chloroform-n-hexane)

출처 및 근거

ORD 기록
ord-fc2d23a0f92643dc96bfca53f297a996
출처 데이터셋
uspto-grants-1996_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05576324

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