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Diethyl Ether → HCID 21223275, 화합물

HRID 1939143
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HRID 1939143 반응식
[Cr](Cl)([O-])(=O)=O.[NH+]1C=CC=CC=1.[OH:12][CH2:13][C:14]1[O:19][CH2:18][N:17]([C:20]([CH3:28])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH3:21])[C:16](=[O:29])[C:15]=1[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1.CCOCC>ClCCl>[CH:13]([C:14]1[O:19][CH2:18][N:17]([C:20]([CH3:28])([C:22]2[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=2)[CH3:21])[C:16](=[O:29])[C:15]=1[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)=[O:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 21223285HCID 21223285, 화합물HCID 178418287HCID 178418287, 화합물

생성물 1

HCID 21223275HCID 21223275, 화합물수율 96%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

Pyridinium chlorochromate (4.70 g) was suspended in dichloromethane (20 ml), and a dichloromethane solution (27 ml) of 6-hydroxymethyl-3-(1-methyl-1-phenylethyl)-5-phenyl-2,3-dihydro-4H-1,3-oxazin-4-one (Compound No. 53, 4.70 g) was added thereto at room temperature. After stirring for about 9 hours, a large amount of ether was added and separated by decantation. The organic layer was dried with magnesium sulfate and the solvent was evaporated. The crude product was purified by silica gel chromatography to afford the captioned compound (4.47 g, yield 96%).

후처리

  1. customat room temperature
  2. customseparated by decantation
  3. dry with materialThe organic layer was dried with magnesium sulfate
  4. customthe solvent was evaporated
  5. customThe crude product was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-31df65bbf3e54447a5c4265f3cddb28f
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05696054

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