Potassium Carbonate → 6-Fluoro-3-methylimidazo[1,2-a]pyridin-2-amine

HRID 1473962노트

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HRID 1473962 반응식
FC(F)(F)C([NH:5][C:6]1[N:7]=[C:8]2[CH:13]=[CH:12][C:11]([F:14])=[CH:10][N:9]2[C:15]=1[CH3:16])=O.C(=O)([O-])[O-].[K+].[K+]>CO.O>[F:14][C:11]1[CH:12]=[CH:13][C:8]2[N:9]([C:15]([CH3:16])=[C:6]([NH2:5])[N:7]=2)[CH:10]=1

참가 물질

5

반응물 2

HCID 11430Potassium CarbonateHCID 576074742,2,2-trifluoro-N-(6-fluoro-3-methylimidazo[1,2-a]pyridin-2-yl)acetamide

생성물 1

HCID 576074616-Fluoro-3-methylimidazo[1,2-a]pyridin-2-amine

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
100 °C

실험 절차

2,2,2-trifluoro-N-(6-fluoro-3-methylimidazo[1,2-a]pyridin-2-yl)acetamide (0.188 g, 0.00072 mol) was dissolved in methanol (4.0 mL) and water (0.5 mL). Potassium carbonate (0.40 g, 0.0029 mol) was added and heated in the microwave for 45 min at 100° C. The solvent concentrated and residue was partitioned between water (50 mL) and ethyl acetate (50 mL). The layers were separated and the organic layer was dried (magnesium sulfate) then chromatographed on silica (55:40:5, DCM:acetonitrle:MeOH) to give 6-fluoro-3-methylimidazo[1,2-a]pyridin-2-amine Rf 0.47, (55:40:5, DCM:acetonitrle:MeOH); MS m/z 166 (M+H).

후처리

  1. concentrationThe solvent concentrated
  2. customresidue was partitioned between water (50 mL) and ethyl acetate (50 mL)
  3. customThe layers were separated
  4. dry with materialthe organic layer was dried (magnesium sulfate)
  5. customthen chromatographed on silica (55:40:5, DCM:acetonitrle:MeOH)

출처 및 근거

ORD 기록
ord-e5f6b5e57c004d96b537fbfa0755dfe3
출처 데이터셋
uspto-grants-2015_04
특허 번호
US09018208B2

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