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Ethyl Acetate → HCID 22676901、化合物

HRID 1006314
ノート
印刷プレビュー

反応式

HRID 1006314 の反応式
[CH2:1]([C:3]1[CH:12]=[CH:11][CH:10]2[CH:5]([C:6](=[O:16])[C:7]([C:13]([OH:15])=[O:14])=[CH:8][O:9]2)[CH:4]=1)[CH3:2].[CH2:17]([C:19]1[CH:20]=[C:21]2[C:26](=[CH:27][CH:28]=1)[O:25][CH:24]=[C:23](C=O)[C:22]2=[O:31])[CH3:18].[OH:32]OS([O-])=O.[K+].CCOC(C)=O>CN(C=O)C>[CH2:1]([C:3]1[CH:12]=[CH:11][CH:10]2[CH:5]([C:6](=[O:16])[C:7]([C:13]([OH:15])=[O:14])=[CH:8][O:9]2)[CH:4]=1)[CH3:2].[CH2:17]([C:19]1[CH:28]=[CH:27][CH:26]2[CH:21]([C:22](=[O:31])[C:23]([OH:32])=[CH:24][O:25]2)[CH:20]=1)[CH3:18]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8857Ethyl AcetateHCID 27588496-Ethyl-3-formylchromoneHCID 22676903HCID 22676903、化合物HCID 23707502Potassium hydroxy sulfite

生成物 2

HCID 22676901HCID 22676901、化合物HCID 22676903HCID 22676903、化合物

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

To prepare 6-ethyl-4-oxo-4a,8a-dihydro-4H-chromene-3-carboxylic acid, 6-ethyl-3-formyl chromone (0.25 g) was dissolved in DMF (10 mL), and OXONE (0.76 g) was added and stirred at room temperature for 3 hours with the reaction having a final volume (12 mL). The reaction was monitored by TLC or GC analysis. EtOAc was added to extract the products and 1N HCl was used to dissolve the salts. The organic extract was washed with 1N HCl (30 mL×3) and brine (30 mL), dried over Na2SO4, and the solvent was removed under reduced pressure to obtain 6-ethyl-4-oxo-4a,8a-dihydro-4H-chromene-3-carboxylic acid in 52% yield and 6-ethyl-3-hydroxy-4a,8a-dihydro-chromene-4-one in 34% yield after purification by silica gel column chromatography.

後処理

  1. extractionto extract the products and 1N HCl
  2. dissolutionto dissolve the salts
  3. extractionThe organic extract
  4. washwas washed with 1N HCl (30 mL×3) and brine (30 mL)
  5. dry with materialdried over Na2SO4
  6. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-c16e355a8281464fab3f8c305bce874c
出典データセット
uspto-grants-2004_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06787671B2

反応ノート

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