Methyl iodide → HCID 57742132、化合物

HRID 660321ノート

反応式

HRID 660321 の反応式
[CH2:1]([O:3][C:4](=[O:16])[CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][O:14][CH3:15])[CH:7]=1)[CH3:2].[H-].[Na+].I[CH3:20]>CN(C=O)C>[CH2:1]([O:3][C:4](=[O:16])[CH:5]([C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([O:12][CH2:13][O:14][CH3:15])[CH:7]=1)[CH3:20])[CH3:2]

参加物

5

反応物 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 57742154HCID 57742154、化合物

生成物 1

HCID 57742132HCID 57742132、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of (3-Methoxymethoxy-phenyl)-acetic acid ethyl ester (31.2 g) in DMF (200 mL) was slowly added sodium hydride (6.21 g) and iodomethane (22.3 g) at 0°. After stirred for 20 h at 0°, this reaction mixture was quenched with water. This mixture was extracted with EtOAc, and combined organic layer was dried over magnesium sulfate, filtered and concentrated in vacuo. The resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1) to afford the product as colorless oil.

後処理

  1. customat 0°
  2. customthis reaction mixture was quenched with water
  3. extractionThis mixture was extracted with EtOAc
  4. dry with materialwas dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe resulting residue was chromatographed on silica gel (n-Hex:EtOAc=10:1)

出典と根拠

ORDレコード
ord-7e16d92d5dfd4d97a3f2dd8ed40c00ae
出典データセット
uspto-grants-2011_12
特許番号
US08084484B2

反応ノート

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