Methanol → 5-Ethynyl-6-methylpyridin-2-amine

HRID 78195

反応式

HRID 78195 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([NH2:8])[CH:5]=[CH:4][C:3]=1[C:9]#[C:10][Si](C)(C)C.CO.C(=O)([O-])[O-].[K+].[K+]>O>[C:9]([C:3]1[CH:4]=[CH:5][C:6]([NH2:8])=[N:7][C:2]=1[CH3:1])#[CH:10]

参加物

5

反応物 3

HCID 887MethanolHCID 11430Potassium CarbonateHCID 592552326-Methyl-5-trimethylsilanylethynyl-pyridin-2-ylamine

生成物 1

HCID 552859385-Ethynyl-6-methylpyridin-2-amine収率 88%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 6-methyl-5-trimethylsilanylethynyl-pyridin-2-ylamine (450 mg, 1.9 mmol) described in Manufacturing Example 187-1-1 and methanol (5 mL) was added potassium carbonate (390 mg, 2.8 mmol), which was stirred for 30 minutes at the same temperature. Water was added to the reaction mixture, which was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium chloride, and was concentrated under a reduced pressure. The residue was purified by silica gel column chromatography (heptane:ethyl acetate=1:1) to obtain the title compound (220 mg, 88%).

後処理

  1. extractionwas extracted with ethyl acetate
  2. washThe organic layer was washed with saturated aqueous sodium chloride
  3. concentrationwas concentrated under a reduced pressure
  4. customThe residue was purified by silica gel column chromatography (heptane:ethyl acetate=1:1)

出典と根拠

ORDレコード
ord-0106c4cd6f4b4a95b3cae1e3d2faafcc
出典データセット
uspto-grants-2014_09
特許番号
US08841327B2

関連ノート

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