Methyl 4-[methoxy(methyl)carbamoyl]benzoate → Methyl 4-butyrylbenzoate

HRID 1914270노트

반응식

HRID 1914270 반응식
[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:15]=[CH:14][C:7]([C:8](N(OC)C)=[O:9])=[CH:6][CH:5]=1.[CH2:17]([Mg]Cl)[CH2:18][CH3:19]>C1COCC1>[CH3:1][O:2][C:3](=[O:16])[C:4]1[CH:5]=[CH:6][C:7]([C:8](=[O:9])[CH2:17][CH2:18][CH3:19])=[CH:14][CH:15]=1

참가 물질

4

반응물 2

HCID 54447022Methyl 4-[methoxy(methyl)carbamoyl]benzoateHCID 178455855HCID 178455855, 화합물

생성물 1

HCID 23143286Methyl 4-butyrylbenzoate수율 23.8%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of N-methoxy-N-methyl-terephthalamic acid methyl ester (4.56 g, 20.4 mmol) in THF (100 mL) is added PrMgCl (2.0M, 30.6 mmol) at 0° C., the reaction is warmed to room temperature, stirred overnight, quenched by NH4Cl aqueous solution, extracted with ethyl acetate. The combined organic layers are washed with brine, dried over sodium sulfate, concentrate. Column chromatography on silica gel gives the title compound (1 g, 23.7%).

후처리

  1. customquenched by NH4Cl aqueous solution
  2. extractionextracted with ethyl acetate
  3. washThe combined organic layers are washed with brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrate

출처 및 근거

ORD 기록
ord-344489e4489d4a84ba0f104678d8005c
출처 데이터셋
uspto-grants-2013_12
특허 번호
US08609892B2

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