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Potassium Carbonate → HCID 18918773, 화합물

HRID 1290793
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반응식

HRID 1290793 반응식
[CH3:1][O:2][C:3]1[CH:12]=[CH:11][CH:10]=[C:9]2[C:4]=1[CH2:5][CH2:6][C:7](=[CH:14]OC)[C:8]2=O.S(O)(O)(=O)=O.[CH3:22][S:23][C:24](=[NH:26])[NH2:25].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[CH3:1][O:2][C:3]1[C:4]2[CH2:5][CH2:6][C:7]3[CH:14]=[N:25][C:24]([S:23][CH3:22])=[N:26][C:8]=3[C:9]=2[CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 752702-Methyl-2-thiopseudourea sulfateHCID 54241815HCID 54241815, 화합물

생성물 1

HCID 18918773HCID 18918773, 화합물수율 72.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 5-methoxy-2-methoxymethylene-1-tetralone (9.78 g) in tetrahydrofuran (200 ml) was added 2-methyl-2-thiopseudourea sulfate (8.34 g), followed by potassium carbonate (9.7 g), and the mixture was refluxed overnight. Solvent was then removed under reduced pressure, the residue stirred with diethyl ether, and filtered. Concentration of the filtrate gave a brown solid, which upon crystallization from ethanol gave 7-methoxy-2-methylthio-5,6-dihydrobenzo[h]quinazoline (8.3 g) as a light brown solid.

후처리

  1. temperaturethe mixture was refluxed overnight
  2. customSolvent was then removed under reduced pressure
  3. filtrationfiltered
  4. customConcentration of the filtrate gave a brown solid, which
  5. customupon crystallization from ethanol

출처 및 근거

ORD 기록
ord-6232eb2c56db4e5190957424a5107e38
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05753663

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