3-Hydroxybenzaldehyde → 3-Isopropoxybenzaldehyde

HRID 594269

反応式

HRID 594269 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6].I[CH:11]([CH3:13])[CH3:12].C([O-])([O-])=O.[K+].[K+].C([O-])([O-])=O.[Cs+].[Cs+]>CN(C=O)C.CCOCC>[CH:11]([O:1][C:2]1[CH:3]=[C:4]([CH:7]=[CH:8][CH:9]=1)[CH:5]=[O:6])([CH3:13])[CH3:12]

参加物

7

反応物 4

HCID 1013-HydroxybenzaldehydeHCID 6362Isopropyl iodideHCID 10796Cesium carbonateHCID 11430Potassium Carbonate

生成物 1

HCID 7129143-Isopropoxybenzaldehyde

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of commercially available 3-hydroxybenzaldehyde (3.000 g; 24.60 mmol), 2-iodopropane (12.528 g; 73.70 mmol), K2CO3 (6.790 g; 49.10 mmol), and Cs2CO3 (1.601 g; 4.91 mmol) in anh. DMF (60 ml) was stirred at rt, under nitrogen, for 17 h. Et2O was added and the organic layer was washed with water, dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure affording 3-isopropoxybenzaldehyde as a yellow oil. LC-MS (conditions A): tR=0.76 min.; [M+H]+: 165.24 g/mol.

後処理

  1. washthe organic layer was washed with water
  2. dry with materialdried over anh. MgSO4
  3. filtrationfiltered
  4. concentrationconcentrated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-2fc9255129084ec1a5ce6a309044e9cd
出典データセット
uspto-grants-2016_01
特許番号
US09242970B2

関連ノート

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