Sodium Hydroxide → HCID 69795215, 화합물

HRID 2181661노트

반응식

HRID 2181661 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 69795215HCID 69795215, 화합물수율 289.3%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매2회

실험 절차

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)+.

후처리

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

출처 및 근거

ORD 기록
ord-dfd74f79afd14164b8f2737a18ad798c
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06894042B2

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