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

HRID 9725노트

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HRID 9725 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

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온도
0 °C

실험 절차

1.5 g 4-Methylamino-2-methylsulfanyl-pyrimidine-5-carbaldehyde were dissolved in 30 ml THF and 14 ml of a 1.4 M solution of methyl magnesium bromide in ether were added dropwise 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-c30e63ee47dc475e94aad2aa23ea7648
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091345B2

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