3-Ethoxy-2-methylacrylaldehyde → (6-Methyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-yl)methanol

HRID 859622

반응식

HRID 859622 반응식
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([CH2:7][OH:8])[N:3]=1.CCO/[CH:12]=[C:13](/[CH:15]=O)\[CH3:14]>C(O)(=O)C>[CH3:15][C:13]1[CH:12]=[N:1][C:2]2[N:6]([N:5]=[C:4]([CH2:7][OH:8])[N:3]=2)[CH:14]=1

참가 물질

4

반응물 2

HCID 30848683-Ethoxy-2-methylacrylaldehydeHCID 178508559HCID 178508559, 화합물

생성물 1

HCID 58762279(6-Methyl-[1,2,4]triazolo[1,5-a]pyrimidin-2-yl)methanol

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
80 °C

실험 절차

To a slurry of (5-amino-1H-[1,2,4]triazol-3-yl)-methanol (16.6 g, 87.6 mmol) from step 6 of example A(1) in acetic acid was added 3-ethoxymethacrolein (10 g, 87.6 mmol). The mixture was heated to 80° C. for 4 hours. Upon cooling of the reaction, the product cyrstallized out of solution. The collected product was awhite solid (14 g, 92%). 1H NMR (300 MHz, DMSO-d6): δ 2.38 (s, 3 H), 4.63 (s, 2 H), 5.52 (s, 1 H), 8.75 (s, 1 H), 9.21 (s, 1 H).

후처리

  1. temperatureUpon cooling of the reaction

출처 및 근거

ORD 기록
ord-397600b6fbae4a279237d05e411ac914
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07151105B2

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