Sodium Hydroxide → 2-(4-Methylsulfonylbenzyl)malonic acid

HRID 526837ノート

反応式

HRID 526837 の反応式
[CH3:1][S:2]([C:5]1[CH:21]=[CH:20][C:8]([CH2:9][CH:10]2[C:15](=[O:16])[O:14]C(C)(C)[O:12][C:11]2=[O:19])=[CH:7][CH:6]=1)(=[O:4])=[O:3].[OH-].[Na+]>>[CH3:1][S:2]([C:5]1[CH:6]=[CH:7][C:8]([CH2:9][CH:10]([C:11]([OH:19])=[O:12])[C:15]([OH:16])=[O:14])=[CH:20][CH:21]=1)(=[O:3])=[O:4]

参加物

3

反応物 2

HCID 14798Sodium HydroxideHCID 867155855-(4-Methylsulfonylbenzyl)-2,2-dimethyl-1,3-dioxane-4,6-dione

生成物 1

HCID 867155862-(4-Methylsulfonylbenzyl)malonic acid

実験手順

A solution of 5-(4-methylsulfonylbenzyl)-2,2-dimethyl-1,3-dioxane-4,6-dione (1.50 g, 4.80 mmol, Intermediate 6: step a) and 3 M aqueous NaOH (16 mL) was heated in the microwave at 75 W for 20 minutes at 120° C. The aqueous mixture was extracted with EtOAc (1×). The aqueous layer was acidified to pH 1 with concentrated aqueous HCl and extracted with EtOAc (2 x). The combined EtOAc extracts was washed with H2O, brine, dried over Na2SO4, filtered and evaporated to dryness to afford the title compound as a white solid.

後処理

  1. extractionThe aqueous mixture was extracted with EtOAc (1×)
  2. extractionextracted with EtOAc (2 x)
  3. washThe combined EtOAc extracts was washed with H2O, brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated to dryness

出典と根拠

ORDレコード
ord-f63fe2d1d9c44b87b4c16ea7630ec059
出典データセット
uspto-grants-2016_05
特許番号
US09346782B2

反応ノート

読み込み中…