Potassium Carbonate → 3-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde

HRID 1958860ノート

反応式

HRID 1958860 の反応式
[OH:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].[CH3:12][C:13]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:14]=1[CH2:15]Cl.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.CCOC(C)=O>[CH3:12][C:13]1[CH:20]=[CH:19][CH:18]=[C:17]([CH3:21])[C:14]=1[CH2:15][O:1][C:2]1[C:3]([O:10][CH3:11])=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 2211542,6-Dimethylbenzyl ChlorideHCID 118049533-Hydroxy-2-methoxybenzaldehyde

生成物 1

HCID 866570083-(2,6-Dimethylbenzyloxy)-2-methoxybenzaldehyde

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The solution of 3-hydroxy-2-methoxybenzaldehyde (5.06 g, 32.7 mmol), 2,6-Dimethylbenzyl chloride (5.04 g, 33.1 mmol) and K2CO3(4.78 g, 34.6 mmol) in dry DMF (15 ml) was stirred at room temperature under argon for 16 hours, then diluted with EtOAc (40 ml), and washed with water 120 ml). The organic layer was concentrated, and purified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1) to give the title compound as an off white solid.

後処理

  1. washwashed with water 120 ml)
  2. concentrationThe organic layer was concentrated
  3. custompurified by flash chromatography on a silica gel column (hex:ethyl acetate 4:1)

出典と根拠

ORDレコード
ord-f27b9eaba72143838fabe56b8aab0a74
出典データセット
uspto-grants-2013_04
特許番号
US08410154B2

反応ノート

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