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Acetone → HCID 22648768, 화합물

HRID 393158
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HRID 393158 반응식
[CH:1]([C:4]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)=[O:5])([CH3:3])[CH3:2].CC(C)=O>C(O)C>[OH:5][CH:4]([C:6]1[C:7]([C:12]([F:15])([F:14])[F:13])=[N:8][CH:9]=[N:10][CH:11]=1)[CH:1]([CH3:2])[CH3:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 180AcetoneHCID 22648741HCID 22648741, 화합물

생성물 1

HCID 22648768HCID 22648768, 화합물수율 87%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

25 g (115 mmol) of 5-isopropylcarbonyl-4-trifluorometylpyrimidine was dissolved in 100 ml of ethanol, and under cooling with ice, 6 g (69 mmol) of a borane-tert-butylamine complex was added, followed by stirring for 2 hours. Further, 20 ml of acetone was added, followed by stirring for 0.5 hour. The solvent was distilled off under reduced pressure, and the residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=1:1) to obtain 22 g (yield: 87%) of 5-(1-hydroxy-2-methylpropyl)-4-trifluoromethylpyrimidine as slightly yellow liquid (nD20=1.4481)

후처리

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  1. temperatureunder cooling with ice, 6 g (69 mmol) of a borane-tert-butylamine complex
  2. additionwas added
  3. stirringby stirring for 0.5 hour
  4. distillationThe solvent was distilled off under reduced pressure
  5. customthe residue was purified by silica gel column chromatography (developing solvent/n-hexane:ethyl acetate=1:1)

출처 및 근거

ORD 기록
ord-3ae17014e7cf4fd08e595c793e9019b8
출처 데이터셋
uspto-grants-2004_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06806230B1

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