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 1521710ノート

反応式

HRID 1521710 の反応式
[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

参加物

4

反応物 2

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

生成物 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 acid収率 54%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
60 °C

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-9c047bfda447435b98bc523810be7759
出典データセット
uspto-grants-2015_07
特許番号
US09073926B2

反応ノート

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