Potassium Carbonate → 10-Methyl-6-oxo-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylic acid

HRID 1521710노트

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HRID 1521710 반응식
[NH2:1][CH2:2][CH2:3][CH:4]([N:6]1[C:10]2=[N:11][C:12]([C:15]([O:17]CC)=[O:16])=[CH:13][CH:14]=[C:9]2[CH:8]=[C:7]1[C:20]([O:22]CC)=O)[CH3:5].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[CH3:5][CH:4]1[N:6]2[C:10]3[N:11]=[C:12]([C:15]([OH:17])=[O:16])[CH:13]=[CH:14][C:9]=3[CH:8]=[C:7]2[C:20](=[O:22])[NH:1][CH2:2][CH2:3]1

참가 물질

4

반응물 2

HCID 11430Potassium CarbonateHCID 67237898Diethyl 1-(4-aminobutan-2-yl)-1H-pyrrolo[2,3-b]pyridine-2,6-dicarboxylate

생성물 1

HCID 6723721510-Methyl-6-oxo-7,8,9,10-tetrahydro-6H-pyrido[3',2':4,5]pyrrolo[1,2-a][1,4]diazepine-2-carboxylic acid수율 54%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
60 °C

실험 절차

To a solution of diethyl 1-(4-aminobutan-2-yl)-1H-pyrrolo[2,3-b]pyridine-2,6-dicarboxylate (1.20 g, 3.60 mmol) in ethanol (35 mL) is added potassium carbonate (1.49 g, 10.8 mmol). The mixture is stirred at 60° C. for 16 h and is then cooled to room temperature. The ethanol is removed in vacuo and the aqueous mixture is acidified to pH 5 with 1N hydrochloric acid and is extracted with ethyl acetate. The combined organic phases are washed with brine, and are dried (Na2SO4) and concentrated in vacuo to afford the title compound as a yellow solid (500 mg, 54%). LCMS: (M+H+).

후처리

  1. temperatureis then cooled to room temperature
  2. customThe ethanol is removed in vacuo
  3. extractionis extracted with ethyl acetate
  4. washThe combined organic phases are washed with brine
  5. dry with materialare dried (Na2SO4)
  6. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-9c047bfda447435b98bc523810be7759
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09073926B2

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