HCID 67785949、化合物 → HCID 19391062、化合物

HRID 1756695ノート

反応式

HRID 1756695 の反応式
[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]

参加物

4

反応物 2

HCID 67785949HCID 67785949、化合物HCID 67786136HCID 67786136、化合物

生成物 1

HCID 19391062HCID 19391062、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6e7dc42316f54c4b87ef7b4f33025a91
出典データセット
uspto-grants-1995_08
特許番号
US05441984

反応ノート

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