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Sulfamic Acid → 6,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

HRID 1105530
ノート
印刷プレビュー

反応式

HRID 1105530 の反応式
[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([CH:23]=[O:24])[C:10]2=[O:25])=[O:5])[CH3:2].S(=O)(=O)([OH:28])N.Cl([O-])=O.[Na+]>ClCCl.O>[CH2:1]([O:3][C:4]([O:6][C:7]1[CH:8]=[C:9]2[C:14](=[CH:15][C:16]=1[O:17][C:18]([O:20][CH2:21][CH3:22])=[O:19])[O:13][CH:12]=[C:11]([C:23]([OH:28])=[O:24])[C:10]2=[O:25])=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 5987Sulfamic AcidHCID 128006236,7-Bis(ethoxycarbonyloxy)chromone-3-carboxaldehydeHCID 23668197Sodium Chlorite

生成物 1

HCID 128006246,7-Bis(ethoxycarbonyloxy)chromone-3-carboxylic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 6344Dichloromethane
溶媒

実験手順

The compound (1.05 g) obtained in (b) of Example 1 was dissolved in 31.5 ml of dichloromethane, and a solution of 1.05 g of sulfamic acid in 18.9 ml of water was added at 10° C. with stirring. Then, a solution of 525.6 mg of sodium chlorite in 1.2 ml of water was added. The solution was stirred at the same temperature for 1 hour, and allowed to separate. The dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and dried over magnesium sulfate. The solvent was distilled off, and ethyl ether was added to the residue to solidify it. The solidified product was collected by filtration, and dried to afford 950 mg of the desired product.

後処理

  1. stirringThe solution was stirred at the same temperature for 1 hour
  2. customto separate
  3. washThe dichloromethane layer was washed with water (once) and then with a saturated aqueous solution of sodium chloride (twice), and
  4. dry with materialdried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. additionethyl ether was added to the residue
  7. filtrationThe solidified product was collected by filtration
  8. customdried

出典と根拠

ORDレコード
ord-5b49a8e31e7546e39db5b65e31c7ec08
出典データセット
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04309354

反応ノート

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