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Dimethylformamide → HCID 58386652, 화합물

HRID 74541
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HRID 74541 반응식
C(N1[C:12]2[C:7](=[C:8]([F:14])[C:9]([F:13])=[CH:10][CH:11]=2)[CH2:6]C1=O)(=O)C.[H-].[Na+].I[CH3:19].[CH3:20][N:21]([CH:23]=[O:24])C>>[F:13][C:9]1[C:8]([F:14])=[CH:7][CH:6]=[C:20]2[C:10]=1[C:11]([CH3:12])([CH3:19])[C:23](=[O:24])[NH:21]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 58386747HCID 58386747, 화합물

생성물 1

HCID 58386652HCID 58386652, 화합물

실험 절차

0.50 g (2.4 mmol) 1-acetyl-4,5-difluoro-1,3-dihydro-indol-2-one were placed in 10 mL DMF under argon. 0.22 g (5.1 mmol) sodium hydride (55%) were added at 0° C. and the reaction mixture was stirred for 1 h. Then 0.32 mL (5.1 mmol) iodomethane were added dropwise. The reaction mixture was stirred overnight at RT, poured onto water and extracted with EtOAc. The organic phase was dried, filtered and concentrated to dryness by rotary evaporation. The residue was purified by HPLC. The product-containing fractions were combined and concentrated to dryness by rotary evaporation.

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후처리

  1. stirringThe reaction mixture was stirred overnight at RT
  2. additionpoured onto water
  3. extractionextracted with EtOAc
  4. customThe organic phase was dried
  5. filtrationfiltered
  6. concentrationconcentrated to dryness by rotary evaporation
  7. customThe residue was purified by HPLC
  8. concentrationconcentrated to dryness by rotary evaporation

출처 및 근거

ORD 기록
ord-0e4565496f7944c39d13adfff8d6afd9
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08829006B2

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