Methanol → Methyl 3-oxocyclohexane-1-carboxylate

HRID 521177

반응식

HRID 521177 반응식
[O:1]=[C:2]1[CH2:7][CH2:6][CH2:5][CH:4]([C:8]([OH:10])=[O:9])[CH2:3]1.[Si](C=[N+]=[N-])(C)(C)[CH3:12].CO>C(OCC)C>[O:1]=[C:2]1[CH2:7][CH2:6][CH2:5][CH:4]([C:8]([O:10][CH3:12])=[O:9])[CH2:3]1

참가 물질

5

반응물 3

HCID 887MethanolHCID 167693TrimethylsilyldiazomethaneHCID 27602523-Oxocyclohexane-1-carboxylic acid

생성물 1

HCID 566099Methyl 3-oxocyclohexane-1-carboxylate

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

To a solution of 3-oxocyclohexanecarboxylic acid (1.0 g, 7.0 mmol) in diethyl ether (28 mL) was added dropwise TMS-diazomethane (3.5 mL, 7.0 mmol, 2.0 mL in diethyl ether). MeOH (30 mL) was added and the mixture was maintained at ambient temperature for 30 minutes. The mixture was concentrated in vacuo, and the residue was purified by MPLC on silica gel (using a gradient elution of 0-45% EtOAc/hexanes). Desired fractions were identified, combined, and concentrated in vacuo to afford the title compound.

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by MPLC on silica gel (
  3. washa gradient elution of 0-45% EtOAc/hexanes)
  4. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-331e63e2801142b8af421c08c9574e82
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09328099B2

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