Diethyl Ether → 3,6-Difluoro-2-methoxybenzaldehyde

HRID 594268ノート

反応式

HRID 594268 の反応式
[F:1][C:2]1[C:3]([OH:11])=[C:4]([C:7]([F:10])=[CH:8][CH:9]=1)[CH:5]=[O:6].IC.[C:14]([O-])([O-])=O.[K+].[K+].CCOCC>CN(C=O)C>[F:1][C:2]1[C:3]([O:11][CH3:14])=[C:4]([C:7]([F:10])=[CH:8][CH:9]=1)[CH:5]=[O:6]

参加物

6

反応物 4

HCID 3283Diethyl EtherHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 225078443,6-Difluoro-2-hydroxybenzaldehyde

生成物 1

HCID 269850393,6-Difluoro-2-methoxybenzaldehyde

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
80 °C

実験手順

A mixture of commercially available 3,6-difluoro-2-hydroxybenzaldehyde (2.450 g; 15.50 mmol), iodomethane (2.199 g; 15.50 mmol), and K2CO3 (2.570 g; 18.60 mmol) in anh. DMF (50 ml) was heated to 80° C., under nitrogen, for 4 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 3,6-difluoro-2-methoxybenzaldehyde as a colorless solid. LC-MS (conditions A): tR=0.62 min.; no ionisation.

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-0d17c2372265451d85a9485686405861
出典データセット
uspto-grants-2016_01
特許番号
US09242970B2

反応ノート

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