Methyl iodide → HCID 85817054, 화합물

HRID 48922노트

반응식

HRID 48922 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 85817054HCID 85817054, 화합물수율 81%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

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%).

후처리

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

출처 및 근거

ORD 기록
ord-57b5a3c0bde84ebdb42b726e30e516f4
출처 데이터셋
uspto-grants-2004_03
특허 번호
US06706698B2

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