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

HRID 1438200ノート

反応式

HRID 1438200 の反応式
[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

参加物

4

反応物 2

HCID 30848683-Ethoxy-2-methylacrylaldehydeHCID 178508559HCID 178508559、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

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 a white solid (14 g, 92%). 1H NMR (300 MHz, DMSO-d6): δ 2.38 (s, 3H), 4.63 (s, 2H), 5.52 (s, 1H), 8.75 (s, 1H), 9.21 (s, 1H).

後処理

  1. temperatureUpon cooling of the reaction

出典と根拠

ORDレコード
ord-9f52f7b1ffaa41ef83079fcd03522288
出典データセット
uspto-grants-2009_11
特許番号
US07622605B2

反応ノート

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