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Dimethylformamide → HCID 21223277, 화합물

HRID 1939142
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HRID 1939142 반응식
[H-].[Na+].[CH3:3]N(C)C=O.[OH:8][CH2:9][C:10]1[O:15][CH2:14][N:13]([C:16]([CH3:24])([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH3:17])[C:12](=[O:25])[C:11]=1[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1.CI>O>[CH3:3][O:8][CH2:9][C:10]1[O:15][CH2:14][N:13]([C:16]([CH3:17])([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH3:24])[C:12](=[O:25])[C:11]=1[C:26]1[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 21223285HCID 21223285, 화합물

생성물 1

HCID 21223277HCID 21223277, 화합물수율 67%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Sodium hydride (60% in oil, 0.11 g) was suspended in diformaldahyde (2 ml), cooled with ice; then a dimethylformamide solution (6 ml) of 6-hydroxymethyl-3-(1-methyl-1-phenylethyl)-5-phenyl-2,3-dihydro-4H-1,3-oxazin-4-one (Compound No. 53, 0.8 g) was added slowly thereto. After stirring the mixture, methyl iodide (0.71 g) was added, and the mixture was stirred again at room temperature. The reaction mixture was poured into water, and extracted with ethyl acetate. The organic layer was rinsed with saturated saline solution, and dried with magnesium sulfate, and the solvent was evaporated. The crude product was purified by silica gel chromatography to afford the captioned compound (0.56 g, yield 67%).

후처리

  1. temperaturecooled with ice
  2. additionwas added
  3. extractionextracted with ethyl acetate
  4. washThe organic layer was rinsed with saturated saline solution
  5. dry with materialdried with magnesium sulfate
  6. customthe solvent was evaporated
  7. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-ebd89c1eafe243d0aea5375e0c3b9e94
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05696054

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