4-(Methylamino)-2-(methylthio)pyrimidine-5-carbaldehyde → 1-(4-Methylamino-2-methylsulfanyl-pyrimidin-5-yl)-ethanol

HRID 1247651ノート

反応式

HRID 1247651 の反応式
[CH3:1][NH:2][C:3]1[C:8]([CH:9]=[O:10])=[CH:7][N:6]=[C:5]([S:11][CH3:12])[N:4]=1.[CH3:13][Mg]Br>C1COCC1.CCOCC>[CH3:1][NH:2][C:3]1[C:8]([CH:9]([OH:10])[CH3:13])=[CH:7][N:6]=[C:5]([S:11][CH3:12])[N:4]=1

参加物

5

反応物 2

HCID 106075204-(Methylamino)-2-(methylthio)pyrimidine-5-carbaldehydeHCID 178418573HCID 178418573、化合物

生成物 1

HCID 219089781-(4-Methylamino-2-methylsulfanyl-pyrimidin-5-yl)-ethanol

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
0 °C

実験手順

1.5 g 4-Methylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde (prepared according to WO 00/24744) were dissolved in 30 mL THF. 14 mL of a 1.4 M solution of methyl magnesium bromide in ether were added drop-wise below 5° C. After stirring for 1 hr at 0° C., another 14 mL Grignard solution were added within 30 min. Stirring was continued for 30 min at 0° C. and finally at RT for 25 hrs. The mixture was quenched with saturated ammonium chloride solution and extracted with ethyl acetate.

後処理

  1. additionanother 14 mL Grignard solution were added within 30 min
  2. stirringStirring
  3. waitwas continued for 30 min at 0° C. and finally at RT for 25 hrs
  4. customThe mixture was quenched with saturated ammonium chloride solution
  5. extractionextracted with ethyl acetate

出典と根拠

ORDレコード
ord-28015d3f512f4801bacb1890b0d63d0f
出典データセット
uspto-grants-2006_10
特許番号
US07129351B2

反応ノート

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