Triethylamine → HCID 86650597、化合物

HRID 1257409

反応式

HRID 1257409 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:4]=[C:5]([C:9]2[N:10]=[C:11]([CH2:14][NH:15][NH:16][C:17](OC(C)(C)C)=O)[S:12][CH:13]=2)[CH:6]=[CH:7][CH:8]=1.CN(C=[C:30]([C:36](=O)[C:37]([F:40])([F:39])[F:38])[C:31]([O:33][CH2:34][CH3:35])=[O:32])C.C(N(CC)CC)C>C(O)C>[F:38][C:37]([F:39])([F:40])[C:36]1[N:15]([CH2:14][C:11]2[S:12][CH:13]=[C:9]([C:5]3[CH:6]=[CH:7][CH:8]=[C:3]([C:2]([F:1])([F:24])[F:25])[CH:4]=3)[N:10]=2)[N:16]=[CH:17][C:30]=1[C:31]([O:33][CH2:34][CH3:35])=[O:32]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 53979199Butanoic acid, 2-[(dimethylamino)methylene]-4,4,4-trifluoro-3-oxo-, ethyl esterHCID 66939173Tert-butyl 2-({4-[3-(trifluoromethyl)phenyl]-1,3-thiazol-2-yl}methyl)hydrazinecarboxylate

生成物 1

HCID 86650597HCID 86650597、化合物収率 69.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of the compound (0.16 g) obtained in Example 103c, ethyl 2-[(dimethylamino)methylidene]-4,4,4-trifluoro-3-oxobutanoate (0.10 g), triethylamine (0.21 mL) and ethanol (4 mL) was heated under reflux for 16 hr. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in ethyl acetate and saturated brine. The ethyl acetate layer was separated, dried over sodium sulfate, and concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.13 g) as a colorless oil.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 16 hr
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. customThe ethyl acetate layer was separated
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)

出典と根拠

ORDレコード
ord-f032328639a14c0ea6a73d18ced22239
出典データセット
uspto-grants-2013_06
特許番号
US08461348B2

関連ノート

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