Sodium Hydroxide → HCID 69795215、化合物

HRID 2181661ノート

反応式

HRID 2181661 の反応式
[CH:1]([C:3]1[O:4][C:5]2[CH:11]=[C:10]([C:12]([O:14][CH3:15])=[O:13])[CH:9]=[CH:8][C:6]=2[CH:7]=1)=[O:2].[OH:16]P([O-])(O)=O.[K+].[O-]Cl=O.[Na+].[OH-].[Na+]>CS(C)=O.O>[CH3:15][O:14][C:12]([C:10]1[CH:9]=[CH:8][C:6]2[CH:7]=[C:3]([C:1]([OH:16])=[O:2])[O:4][C:5]=2[CH:11]=1)=[O:13]

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 516951Monobasic potassium phosphateHCID 22481722588702-95-8HCID 23668197Sodium Chlorite

生成物 1

HCID 69795215HCID 69795215、化合物収率 289.3%

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 962Water溶媒2 回

実験手順

Methyl 2-formyl-1-benzofuran-6-carboxylate (1.23 g, 6.0 mmol) is dissolved in DMSO (12 ml). KH2PO4 (229 mg, 1.68 mmol) in H2O (2 ml) and NaClO2 (80%, 949 mg, 8.4 mmol) in H2O (12 ml) are added drop-wise to the solution, and the reaction is stirred over the weekend at RT. The pH is adjusted to 10 with 2N NaOH and the mixture is extracted with Et2O (3×50 ml). The pH is adjusted again to 3 with concentrated HCl and the slurry is filtered. The cake is dried overnight, yielding 1.07 g (81%) of 6-(methoxycarbonyl)-1-benzofuran-2-carboxylic acid as an ivory solid. HRMS (FAB) calcd for C11H8O5+H: 221.0450, found 221.0436 (M+H)+.

後処理

  1. extractionthe mixture is extracted with Et2O (3×50 ml)
  2. filtrationthe slurry is filtered
  3. customThe cake is dried overnight

出典と根拠

ORDレコード
ord-dfd74f79afd14164b8f2737a18ad798c
出典データセット
uspto-grants-2005_05
特許番号
US06894042B2

反応ノート

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