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Water → HCID 14648843, 화합물

HRID 1164717
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HRID 1164717 반응식
[H-].[Na+].[CH3:3][O:4][C:5]1[CH:10]=[C:9]([O:11][CH3:12])[N:8]=[C:7]([O:13][C:14]2[CH:15]=[CH:16][CH:17]=[C:18]([OH:29])[C:19]=2[C:20]([O:22][CH2:23][CH2:24][Si:25]([CH3:28])([CH3:27])[CH3:26])=[O:21])[N:6]=1.[Cl:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[N:34]=[C:33](S(C)(=O)=O)[N:32]=1.O>C1COCC1>[Cl:30][C:31]1[CH:36]=[C:35]([O:37][CH3:38])[N:34]=[C:33]([O:29][C:18]2[CH:17]=[CH:16][CH:15]=[C:14]([O:13][C:7]3[N:6]=[C:5]([O:4][CH3:3])[CH:10]=[C:9]([O:11][CH3:12])[N:8]=3)[C:19]=2[C:20]([O:22][CH2:23][CH2:24][Si:25]([CH3:27])([CH3:26])[CH3:28])=[O:21])[N:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 24758Sodium hydrideHCID 137292254-Chloro-2-(methanesulfonyl)-6-methoxypyrimidineHCID 14648842HCID 14648842, 화합물

생성물 1

HCID 14648843HCID 14648843, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

NaH (0.4 g, purity: 60%) was suspended in 50 ml of THF. To this suspension, trimethylsilylethyl 6-(4,6-dimethoxypyrimidin-2-yl)oxysalicylate (3.0 g) was added, and the mixture was stirred at room temperature for 30 minutes. To this mixture, 4-chloro-6-methoxy-2-methylsulfonylpyrimidine (1.8 g) was added, and the mixture was stirred at room temperature for further 12 hours. After completion of the reaction, water was added thereto, and the mixture was extracted with ethyl ether. The ethyl ether layer was dried over anhydrous magnesium sulfate. Then, the solvent was distilled off under reduced pressure. The crude extract thus obtained was purified by silica gel column chromatography to obtain the above identified compound as a slightly yellow liquid (4.0 g).

후처리

  1. stirringthe mixture was stirred at room temperature for further 12 hours
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl ether
  4. dry with materialThe ethyl ether layer was dried over anhydrous magnesium sulfate
  5. distillationThen, the solvent was distilled off under reduced pressure
  6. extractionThe crude extract thus
  7. customobtained
  8. customwas purified by silica gel column chromatography
  9. customto obtain the

출처 및 근거

ORD 기록
ord-bb5a177b201f4d73a007625c66f30d11
출처 데이터셋
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04906285

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