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2-Methoxypropene → 2,2-dimethyl-1-(1-methylethyl)-6-(pyridin-4-yl)-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one

HRID 2363997
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HRID 2363997 반응식
[CH3:1][CH:2]([NH:4][C:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=2)[S:7][C:6]=1[C:16]([NH2:18])=[O:17])[CH3:3].CO[C:21]([CH3:23])=[CH2:22]>C(O)(=O)C>[CH3:3][C:2]1([CH3:1])[N:4]([CH:21]([CH3:23])[CH3:22])[C:5]2[CH:9]=[C:8]([C:10]3[CH:15]=[CH:14][N:13]=[CH:12][CH:11]=3)[S:7][C:6]=2[C:16](=[O:17])[NH:18]1
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참가 물질

4

반응물 2

HCID 83002-MethoxypropeneHCID 667440693-[(1-Methylethyl)amino]-5-(pyridin-4-yl)thiophene-2-carboxamide

생성물 1

HCID 667436222,2-dimethyl-1-(1-methylethyl)-6-(pyridin-4-yl)-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one수율 52%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
35 °C

실험 절차

A mixture of 3-[(1-methylethyl)amino]-5-(pyridin-4-yl)thiophene-2-carboxylic acid (0.225 g, 0.858 mmol), ammonium chloride (0.459 g, 8.58 mmol) and triethylamine (1.21 mL, 8.58 mmol) in DMF (5 mL) was stirred at room temperature for 15 min. To the resulting mixture was added 1-(3-(dimethylamino)propyl)-3-ethyl carbodiimide hydrochloride (0.493 g, 2.57 mmol), and 1-hydroxybenzotriazole (0.347 g, 2.57 mmol) and the reaction was stirred at room temperature for 65 h. Then, the reaction mixture was diluted with sat. NaHCO3 (120 mL) and extracted with ethyl acetate (3×100 mL). The combined organic layers were washed with water (2×50 mL) and brine (100 mL), dried over magnesium sulfate, filtered and concentrated to give crude 3-[(1-methylethyl)amino]-5-(pyridin-4-yl)thiophene-2-carboxamide (0.225 g) as an orange solid. A mixture of 3-[(1-methylethyl)amino]-5-(pyridin-4-yl)thiophene-2-carboxamide (0.105 g) and 2-methoxypropene (1.53 mL, 16.0 mmol) in acetic acid (1.5 mL) was heated at 35° C. overnight. Then, the reaction mixture was cooled to room temperature and concentrated. The obtained residue was dissolved in methanol (10 mL), and the solution was concentrated with NaHCO3 (1 g) and silica gel (5 mL), and the residue was purified by flash chromatography (Combiflash, silica gel, ethyl acetate to 95:5 ethyl acetate /methanol) to give the title compound (0.063 g, 2 step yield 52%) as an orange solid:

후처리

  1. temperatureThen, the reaction mixture was cooled to room temperature
  2. concentrationconcentrated
  3. dissolutionThe obtained residue was dissolved in methanol (10 mL)
  4. concentrationthe solution was concentrated with NaHCO3 (1 g) and silica gel (5 mL)
  5. customthe residue was purified by flash chromatography (Combiflash, silica gel, ethyl acetate to 95:5 ethyl acetate /methanol)

출처 및 근거

ORD 기록
ord-5083ef1332b44a979aa07b5a7c0aca25
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08691828B2

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