Methyl iodide → HCID 85817054、化合物

HRID 48922ノート

反応式

HRID 48922 の反応式
[CH3:1][N:2]([CH3:13])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([OH:12])[CH:5]=1.[CH3:14][I:15]>O1CCOCC1>[I-:15].[CH3:13][N+:2]([CH3:14])([CH3:1])[CH2:3][C:4]1[CH:9]=[CH:8][C:7]([O:10][CH3:11])=[C:6]([OH:12])[CH:5]=1

参加物

4

反応物 2

HCID 6328Methyl iodideHCID 13434502Dimethyl(3-hydroxy-4-methoxybenzyl)amine

生成物 1

HCID 85817054HCID 85817054、化合物収率 81%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

To a dioxane solution (250 ml) of the dimethyl(3-hydroxy-4-methoxybenzyl)amine thus obtained (16 g, 88.5 mmol) was added methyl iodide (8.26 ml, 132 mmol) and the resulting mixture was refluxed for 4 h. The solid formed was filtered and washed with dioxane to yield 23 g (81%) of the trimethyl(3-hydroxy-4-methoxybenzyl) ammonium iodide salt. This latter was suspended in 100 ml xylene, triethyl phosphite (18 ml, 107 mmol) was added and the resulting mixture was refluxed for 16 h. The solid formed was filtered and the solvent and excess of phosphite were evaporated under vacuum to give after short path distillation diethyl (3-hydroxy-4-methoxybenzyl)phosphonate as a viscous oil (4 g, 10%).

後処理

  1. temperaturethe resulting mixture was refluxed for 4 h
  2. customThe solid formed
  3. filtrationwas filtered
  4. washwashed with dioxane

出典と根拠

ORDレコード
ord-57b5a3c0bde84ebdb42b726e30e516f4
出典データセット
uspto-grants-2004_03
特許番号
US06706698B2

反応ノート

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