Triethylamine → 2.5-Di-[(methanesulfonyl)oxy]benzaldehyde

HRID 412162

反応式

HRID 412162 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][C:7]([OH:10])=[CH:6][C:3]=1[CH:4]=[O:5].C(N(CC)CC)C.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>ClCCl>[CH3:18][S:19]([O:1][C:2]1[CH:9]=[CH:8][C:7]([O:10][S:19]([CH3:18])(=[O:21])=[O:20])=[CH:6][C:3]=1[CH:4]=[O:5])(=[O:21])=[O:20]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 709492,5-Dihydroxybenzaldehyde

生成物 1

HCID 185361862.5-Di-[(methanesulfonyl)oxy]benzaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2,5-dihydroxybenzaldehyde (8.22 g, 59.5 mmol) in 100 mL of dichloromethane at 0° C. was added triethylamine (24.8 mL, 178 mmol), followed by dropwise addition of methanesulfonyl chloride (10.1 mL, 130 mmol). After 30 minutes, the solution was concentrated in vacuo, then partitioned between EtOAc and saturated NaHCO3 solution. The organic layer was washed with water and brine, dried (Na2SO4), filtered, and concentrated in vacuo. The product was isolated as a brown oil which was used without further purification.

後処理

  1. concentrationthe solution was concentrated in vacuo
  2. custompartitioned between EtOAc and saturated NaHCO3 solution
  3. washThe organic layer was washed with water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. customThe product was isolated as a brown oil which
  8. customwas used without further purification

出典と根拠

ORDレコード
ord-5623e8b1669c443d8e97930d5d019eb5
出典データセット
uspto-grants-2003_05
特許番号
US06562823B1

関連ノート

読み込み中…