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Dimethylformamide → HCID 59244769, 화합물

HRID 912250
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HRID 912250 반응식
[CH3:1]N(C=O)C.[Br:6][C:7]1[CH:8]=[C:9]([NH:13][C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1.[H-].[Na+].CI>O>[Br:6][C:7]1[CH:8]=[C:9]([N:13]([CH3:1])[C:14](=[O:16])[CH3:15])[CH:10]=[CH:11][CH:12]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 12123N-(3-Bromophenyl)acetamideHCID 24758Sodium hydride

생성물 1

HCID 59244769HCID 59244769, 화합물수율 94%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a DMF solution (15 ml) of N-(3-bromo-phenyl)-acetamide (1.19 g) obtained in Step A, 60% oily sodium hydride (279 mg) was added, followed by stirring at room temperature for 10 minutes. To this, methyl iodide (434 μl) was added, followed by stirring at room temperature for 21 hours. To this, water (30 ml) was added, followed by extraction with ethyl acetate (30 ml×2), and the organic layer was dried over sodium sulfate. The sodium sulfate was filtered off, followed by purification by silica gel column chromatography (dichloromethane/methanol=200/1), to obtain the desired compound (1.20 g, 94%).

후처리

  1. stirringby stirring at room temperature for 21 hours
  2. extractionfollowed by extraction with ethyl acetate (30 ml×2)
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationThe sodium sulfate was filtered off
  5. customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=200/1)

출처 및 근거

ORD 기록
ord-dda48dbea7d743c6b1506fd0214f322c
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022205B2

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