Methyl iodide → HCID 67363339, 화합물

HRID 245756노트

반응식

HRID 245756 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:10]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[NH:8][C:5]2=[N:6][CH:7]=1.[C:15](=O)([O-])[O-].[K+].[K+].IC>[Cl-].[Na+].O>[Cl:1][C:2]1[CH:3]=[C:4]2[CH:10]=[C:9]([C:11]([O:13][CH3:14])=[O:12])[N:8]([CH3:15])[C:5]2=[N:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 45073274Methyl 5-chloro-1H-pyrrolo[2,3-b]pyridine-2-carboxylate

생성물 1

HCID 67363339HCID 67363339, 화합물수율 84.7%

시약·촉매·용매 1

HCID 57417360Sodium chloride; water용매

실험 절차

To a stirred solution of methyl 5-chloro-1H-pyrrolo[2,3-b]pyridine-2-carboxylate (0.986 g, 4.68 mmol) N,N-dimethylformamide (20 ml) at room temperature under a nitrogen atmosphere was added potassium carbonate (0.647 g, 4.68 mmol). After 30 minutes iodomethane (0.321 ml, 5.15 mmol) was added and the resulting mixture was stirred at room temperature overnight. Brine was added and the mixture was extracted with ethyl acetate three times. The combined organic layers were washed with brine, dried (Na2SO4) and concentrated in vacuo. The residue was coated onto hydromatrix and purified by column chromatography (silica gel; heptane/ethyl acetate 4/1) to give methyl 5-chloro-1-methyl-1H-pyrrolo[2,3-b]pyridine-2-carboxylate (0.89 g).

후처리

  1. extractionthe mixture was extracted with ethyl acetate three times
  2. washThe combined organic layers were washed with brine
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated in vacuo
  5. custompurified by column chromatography (silica gel; heptane/ethyl acetate 4/1)

출처 및 근거

ORD 기록
ord-f70d071458a64d8e91ad8f7d10757743
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658794B2

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