Methyl iodide → HCID 90030398, 화합물

HRID 1488190노트

반응식

HRID 1488190 반응식
[CH3:1][Si:2]([CH3:14])([CH3:13])[CH2:3][CH2:4][O:5][CH2:6][N:7]1[CH:11]=[C:10]([OH:12])[CH:9]=[N:8]1.[C:15]([O-])([O-])=O.[Cs+].[Cs+].CI>O1CCCC1>[CH3:15][O:12][C:10]1[CH:9]=[N:8][N:7]([CH2:6][O:5][CH2:4][CH2:3][Si:2]([CH3:14])([CH3:13])[CH3:1])[CH:11]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 900300951-[[2-(Trimethylsilyl)ethoxy]methyl]-1H-pyrazol-4-ol2회

생성물 1

HCID 90030398HCID 90030398, 화합물수율 92%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazol-4-ol (compound 280.2, 2.14 g, 10.0 mmol) in tetrahydrofuran (50 mL) was added Cs2CO3 (6.5 g, 20.0 mmol) in portions. To this was added CH3I (1.25 mL, 20.0 mmol) dropwise. The reaction mixture was stirred for 3 h at room temperature, then concentrated under reduced pressure. The resulting residue was dissolved in 100 mL of EtOAc. The solids were filtered off and the filtrate was concentrated under reduced pressure. This resulted in 2.1 g (92%) of the title compound as a colorless oil.

후처리

  1. concentrationconcentrated under reduced pressure
  2. dissolutionThe resulting residue was dissolved in 100 mL of EtOAc
  3. filtrationThe solids were filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d68de0b0c2634a80bbbf76b013f3678b
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09428502B2

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