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Methyl iodide → HCID 67281758、化合物

HRID 1187501
ノート
印刷プレビュー

反応式

HRID 1187501 の反応式
CI.[CH2:3]([O:10][C:11]1[C:16](=[O:17])[C:15]([CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:14][NH:13][C:12]=1[CH3:23])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[C:24](=O)([O-])[O-].[K+].[K+]>C(#N)C.ClCCl>[CH2:3]([O:10][C:11]1[C:16](=[O:17])[C:15]([CH2:18][C:19]([F:22])([F:21])[F:20])=[CH:14][N:13]([CH3:24])[C:12]=1[CH3:23])[C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 67282712HCID 67282712、化合物

生成物 1

HCID 67281758HCID 67281758、化合物収率 95%

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

Methyl iodide (11 mL, 176 mmol) was added to a suspension of 3-benzyloxy-2-methyl-5-(2,2,2-trifluoro-ethyl)-1H-pyridin-4-one (1.18 g, 4.0 mmol) and potassium carbonate (1.06 g, 7.7 mmol) in acetonitrile (25 mL). The resulting mixture was heated to reflux, and the reaction was completed within 40 min. The mixture was cooled to RT, and the solid particulates was filtered off. The filtrate was concentrated in vacuo to give a solid. The solid was taken up in dichloromethane, and the organic layer was washed with brine, dried over Na2SO4, filtered and concentrated in vacuo to afford 3-benzyloxy-1,2-dimethyl-5-(2,2,2-trifluoro-ethyl)-1H-pyridin-4-one as a colorless oil (1.3 g, 95% yield, HPLC Method 1 (Example 24), RT=15.9 min, HPLC purity (peak percent area): 98% at λ=280 nm).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureto reflux
  3. filtrationthe solid particulates was filtered off
  4. concentrationThe filtrate was concentrated in vacuo
  5. customto give a solid
  6. washthe organic layer was washed with brine
  7. dry with materialdried over Na2SO4
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-76dbc65f78c6406aad199a9549102e40
出典データセット
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08673943B2

反応ノート

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