3-Methylcatechol → 3-Methylveratrole

HRID 71052

反応式

HRID 71052 の反応式
[CH3:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:4]([OH:5])[C:3]=1O.[CH3:10]I.[C:12]([O-:15])([O-])=O.[K+].[K+]>CC(C)=O>[CH3:10][O:5][C:4]1[CH:6]=[CH:7][CH:8]=[C:2]([CH3:1])[C:3]=1[O:15][CH3:12]

参加物

5

反応物 3

HCID 3403-MethylcatecholHCID 6328Methyl iodideHCID 11430Potassium Carbonate

生成物 1

HCID 782153-Methylveratrole

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

In a round bottom flask, 3-methyl catechol (5.0 g, 40.3 mmol), MeI (22.3 g, 157.1 mmol), and K2CO3 (18.9 g, 136.9 mmol) were dissolved in acetone (20.0 ml). The reaction mixture was stirred at room temperature for 1 h, then at 60° C. for overnight. The reaction mixture was concentrated and chromatographed on silica gel using EtOAc/Hexane (5:95). A pale yellow liquid was isolated in 100% (6.13 g). The characterization of the compound matched previous report: Xing, L.; Wang, X.; Cheng, X.; Zhu, R.; Liu, B.; Hu, Y. Tetrahedron Letters 2007, 63, (38), 9382-9386.

後処理

  1. waitat 60° C. for overnight
  2. concentrationThe reaction mixture was concentrated
  3. customchromatographed on silica gel
  4. customA pale yellow liquid was isolated in 100% (6.13 g)

出典と根拠

ORDレコード
ord-5680a16de7274cb5aacf4ba0058eddff
出典データセット
uspto-grants-2014_09
特許番号
US08822720B2

関連ノート

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