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

HRID 1473962ノート

反応式

HRID 1473962 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-e5f6b5e57c004d96b537fbfa0755dfe3
出典データセット
uspto-grants-2015_04
特許番号
US09018208B2

反応ノート

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