Formic Acid → 7-(4-Chlorophenyl)-8-isopropyl-3H-chromeno[7,8-d]imidazol-6-one

HRID 14490

反応式

HRID 14490 の反応式
[NH2:1][C:2]1[C:11]([NH2:12])=[C:10]2[C:5]([C:6](=[O:23])[C:7]([C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)=[C:8]([CH:13]([CH3:15])[CH3:14])[O:9]2)=[CH:4][CH:3]=1.[CH:24](O)=O>C(OCC)(=O)C>[Cl:22][C:19]1[CH:18]=[CH:17][C:16]([C:7]2[C:6](=[O:23])[C:5]3[CH:4]=[CH:3][C:2]4[NH:1][CH:24]=[N:12][C:11]=4[C:10]=3[O:9][C:8]=2[CH:13]([CH3:14])[CH3:15])=[CH:21][CH:20]=1

参加物

4

反応物 2

HCID 284Formic AcidHCID 687024427,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one

生成物 1

HCID 687038007-(4-Chlorophenyl)-8-isopropyl-3H-chromeno[7,8-d]imidazol-6-one

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (43 mg, 0.13 mmol) is dissolved in formic acid (1.5 ml), and the solution is heated at reflux for 1 h. The reaction mixture is cooled to room temperature, diluted with ethyl acetate (40 ml) and washed with saturated sodium bicarbonate solution (2×30 ml), water (40 ml) and saturated brine (30 ml). The organic layer is dried (MgSO4), filtered and evaporated to give a pale yellow solid. This is triturated with n-hexane/ethyl acetate/dichloromethane and filtered to give a colourless powder.

後処理

  1. temperaturethe solution is heated
  2. temperatureat reflux for 1 h
  3. washwashed with saturated sodium bicarbonate solution (2×30 ml), water (40 ml) and saturated brine (30 ml)
  4. dry with materialThe organic layer is dried (MgSO4)
  5. filtrationfiltered
  6. customevaporated
  7. customto give a pale yellow solid
  8. customThis is triturated with n-hexane/ethyl acetate/dichloromethane
  9. filtrationfiltered
  10. customto give a colourless powder

出典と根拠

ORDレコード
ord-8bb1f1e2a9354ba88a777941ab693f2e
出典データセット
uspto-grants-2010_06
特許番号
US07732435B2

関連ノート

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