Trifluoroacetic acid → HCID 57722978、化合物

HRID 1987035ノート

反応式

HRID 1987035 の反応式
[Cl:1][C:2]1[C:7]([CH2:8][CH2:9][C:10]([O:12][C:13](C)(C)C)=[O:11])=[C:6]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[CH:5]=[C:4]([Cl:24])[N:3]=1.FC(F)(F)C(O)=O>C1(OC)C=CC=CC=1>[Cl:1][C:2]1[C:7]([CH2:8][CH2:9][C:10]([O:12][CH3:13])=[O:11])=[C:6]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[Cl:23])[CH:5]=[C:4]([Cl:24])[N:3]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 57722998HCID 57722998、化合物

生成物 1

HCID 57722978HCID 57722978、化合物収率 64.4%

試薬・触媒・溶媒 1

HCID 7519Anisole溶媒

実験手順

tert-Butyl 3-[2,6-dichloro-4-(2-chlorophenyl)-3-pyridinyl]propanoate (2.44 g, 6.31 mmol) was dissolved in anisole (6 ml) and trifluoroacetic acid (30 ml) added and the solution allowed to stand at 21° for 2 h, then evaporated in vacuo. The residue was dissolved in toluene (40 ml)-methanol (10 ml), and a 2M solution of trimethylsilyldiazomethane in hexanes added (8 ml), and the solution allowed to stand for 0.5 h. The solution was evaporated in vacuo, and the resulting oil purified by flash chromatography over silica eluting with cyclohexane-ethyl acetate (100:0-65:35) to give the title compound as a viscous gum (1.40 g, 64%)

後処理

  1. customevaporated in vacuo
  2. dissolutionThe residue was dissolved in toluene (40 ml)-methanol (10 ml)
  3. additiona 2M solution of trimethylsilyldiazomethane in hexanes added (8 ml)
  4. waitto stand for 0.5 h
  5. customThe solution was evaporated in vacuo
  6. customthe resulting oil purified by flash chromatography over silica eluting with cyclohexane-ethyl acetate (100:0-65:35)

出典と根拠

ORDレコード
ord-3711ce8d3fa94adf8430d58378de2b62
出典データセット
uspto-grants-2009_06
特許番号
US07550480B2

反応ノート

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