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

HRID 78195

반응식

HRID 78195 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 552859385-Ethynyl-6-methylpyridin-2-amine수율 88%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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%).

후처리

  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)

출처 및 근거

ORD 기록
ord-0106c4cd6f4b4a95b3cae1e3d2faafcc
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08841327B2

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