Methyl iodide → HCID 90030398、化合物

HRID 1488190ノート

反応式

HRID 1488190 の反応式
[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

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 900300951-[[2-(Trimethylsilyl)ethoxy]methyl]-1H-pyrazol-4-ol2 回

生成物 1

HCID 90030398HCID 90030398、化合物収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d68de0b0c2634a80bbbf76b013f3678b
出典データセット
uspto-grants-2016_08
特許番号
US09428502B2

反応ノート

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