HCID 67785949, 화합물 → HCID 19391062, 화합물

HRID 1756695노트

반응식

HRID 1756695 반응식
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]1[CH:8]=[C:9]([CH:12]=[C:13]([C:19]([CH3:22])([CH3:21])[CH3:20])[C:14]=1[O:15]COC)[CH2:10][NH2:11].[CH3:23][S:24][C:25]1[CH:30]=[CH:29][C:28]([N:31](C2C=CC([N+]([O-])=O)=CC=2)[C:32](=O)[O-:33])=[CH:27][CH:26]=1>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7]1[CH:8]=[C:9]([CH2:10][NH:11][C:32]([NH:31][C:28]2[CH:29]=[CH:30][C:25]([S:24][CH3:23])=[CH:26][CH:27]=2)=[O:33])[CH:12]=[C:13]([C:19]([CH3:21])([CH3:20])[CH3:22])[C:14]=1[OH:15]

참가 물질

4

반응물 2

HCID 67785949HCID 67785949, 화합물HCID 67786136HCID 67786136, 화합물

생성물 1

HCID 19391062HCID 19391062, 화합물수율 61.9%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution of 4.2 g (12.2 mmol) of the compound of Example 3 dissolved in 50 ml of toluene were added 3.70 g (12.2 mmol) of the compound of Example 12. The resulting solution was heated to reflux, stirred at that temperature for 45 minutes and then cooled to room temperature. Any solid particulates which had precipitated upon cooling were removed by filtration and the filtrate was concentrated to dryness to provide a residue. This residue was purified by column chromatography (10-40% ethyl acetate in hexane gradient as eluent) and fractions containing the desired product were combined and concentrated to dryness to provide 3.33 g of title compound.

후처리

  1. temperatureThe resulting solution was heated
  2. temperatureto reflux
  3. customAny solid particulates which had precipitated
  4. temperatureupon cooling
  5. customwere removed by filtration
  6. concentrationthe filtrate was concentrated to dryness
  7. customto provide a residue
  8. customThis residue was purified by column chromatography (10-40% ethyl acetate in hexane gradient as eluent) and fractions
  9. additioncontaining the desired product
  10. concentrationconcentrated to dryness

출처 및 근거

ORD 기록
ord-6e7dc42316f54c4b87ef7b4f33025a91
출처 데이터셋
uspto-grants-1995_08
특허 번호
US05441984

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