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Sodium Bicarbonate → 6-methoxy-7-(3-(N-methyl-N-methylsulphonylamino)propoxy)quinazolin-4-one

HRID 1791652
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HRID 1791652 반응식
BrC1C=CC([O:6][C:7]2[C:16]3[C:11](=[CH:12][C:13]([O:19][CH2:20][CH2:21][CH2:22][N:23]([CH3:28])[S:24]([CH3:27])(=[O:26])=[O:25])=[C:14]([O:17][CH3:18])[CH:15]=3)[N:10]=[CH:9][N:8]=2)=C(F)C=1.C(=O)([O-])O.[Na+]>Cl>[CH3:18][O:17][C:14]1[CH:15]=[C:16]2[C:11](=[CH:12][C:13]=1[O:19][CH2:20][CH2:21][CH2:22][N:23]([CH3:28])[S:24]([CH3:27])(=[O:26])=[O:25])[N:10]=[CH:9][NH:8][C:7]2=[O:6]
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참가 물질

4

반응물 2

HCID 516892Sodium BicarbonateHCID 220307614-(4-Bromo-2-fluorophenoxy)-6-methoxy-7-(3-(N-methyl N-methylsulphonylamino)propoxy)quinazoline

생성물 1

HCID 1357631136-methoxy-7-(3-(N-methyl-N-methylsulphonylamino)propoxy)quinazolin-4-one수율 104%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

4-(4-Bromo-2-fluorophenoxy)-6-methoxy-7-(3-(N-methyl N-methylsulphonylamino)propoxy)quinazoline (4.70 g, 9.1 mmol) was dissolved in 2N aqueous hydrochloric acid solution (85 ml) and heated at reflux for 1 hour. After cooling, the solution was carefully poured into saturated aqueous sodium hydrogen carbonate solution (to pH8) and stirred vigorously for 30 minutes. The resulting precipitate was filtered and dried. The filter cake was then taken up as a suspension in acetone, filtered, washed with diethyl ether and dried to give 6-methoxy-7-(3-(N-methyl-N-methylsulphonylamino)propoxy)quinazolin-4-one (3.23 g, 88%).

후처리

  1. temperatureheated
  2. temperatureat reflux for 1 hour
  3. temperatureAfter cooling
  4. filtrationThe resulting precipitate was filtered
  5. customdried
  6. filtrationfiltered
  7. washwashed with diethyl ether
  8. customdried

출처 및 근거

ORD 기록
ord-cb33bc7bf02042539bf1ac7c3408d1b0
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07074800B1

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