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

HRID 640478

反応式

HRID 640478 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-1c5f081ac53b4007aa60734435df29f6
出典データセット
uspto-grants-2010_04
特許番号
US07691882B2

関連ノート

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