Trifluoroacetic acid → HCID 57722978, 화합물

HRID 1987035노트

반응식

HRID 1987035 반응식
[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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 57722998HCID 57722998, 화합물

생성물 1

HCID 57722978HCID 57722978, 화합물수율 64.4%

시약·촉매·용매 1

HCID 7519Anisole용매

실험 절차

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%)

후처리

  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)

출처 및 근거

ORD 기록
ord-3711ce8d3fa94adf8430d58378de2b62
출처 데이터셋
uspto-grants-2009_06
특허 번호
US07550480B2

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