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

HRID 1247651노트

반응식

HRID 1247651 반응식
[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

참가 물질

5

반응물 2

HCID 106075204-(Methylamino)-2-(methylthio)pyrimidine-5-carbaldehydeHCID 178418573HCID 178418573, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-28015d3f512f4801bacb1890b0d63d0f
출처 데이터셋
uspto-grants-2006_10
특허 번호
US07129351B2

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