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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Sulfamic Acid → 6,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid

HRID 1105532
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인쇄 미리보기

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HRID 1105532 반응식
[Cl:1][C:2]([Cl:31])([Cl:30])[CH2:3][O:4][C:5]([O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[O:18][C:19]([O:21][CH2:22][C:23]([Cl:26])([Cl:25])[Cl:24])=[O:20])[O:14][CH:13]=[C:12]([CH:27]=[O:28])[C:11]2=[O:29])=[O:6].S(=O)(=O)([OH:34])N.Cl([O-])=O.[Na+]>ClCCl.O>[Cl:31][C:2]([Cl:1])([Cl:30])[CH2:3][O:4][C:5]([O:7][C:8]1[CH:9]=[C:10]2[C:15](=[CH:16][C:17]=1[O:18][C:19]([O:21][CH2:22][C:23]([Cl:24])([Cl:25])[Cl:26])=[O:20])[O:14][CH:13]=[C:12]([C:27]([OH:34])=[O:28])[C:11]2=[O:29])=[O:6]
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참가 물질

6

반응물 3

HCID 5987Sulfamic AcidHCID 12800626HCID 12800626, 화합물2회HCID 23668197Sodium Chlorite

생성물 1

HCID 128006276,7-Bis(2,2,2-trichloroethoxycarbonyloxy)chromone-3-carboxylic acid수율 79.4%

시약·촉매·용매 2

HCID 962Water용매2회
HCID 6344
Dichloromethane
용매

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온도
10 °C

실험 절차

The compound (838.4 mg) obtained in Example 4, (b) was dissolved in 16 ml of dichloromethane, and with stirring at 10° C., a solution of 525 mg of sulfamic acid in 9.5 ml of water was added, followed by addition of a solution of 262.8 mg of sodium chlorite in 0.6 ml of water. The mixture was stirred for 1 hour at the same temperature. The reaction mixture was allowed to separate. The dichloromethane layer was washed with water and then with a saturated aqueous solution of sodium chloride, and then dried over magnesium sulfate. The solvent was distilled off, and the residue was recrystallized from ethyl ether to afford 685 mg of the desired product.

후처리

  1. stirringThe mixture was stirred for 1 hour at the same temperature
  2. customto separate
  3. washThe dichloromethane layer was washed with water
  4. dry with materialwith a saturated aqueous solution of sodium chloride, and then dried over magnesium sulfate
  5. distillationThe solvent was distilled off
  6. customthe residue was recrystallized from ethyl ether

출처 및 근거

ORD 기록
ord-2c8177ac15f6412393598f20ba15eb47
출처 데이터셋
uspto-grants-1982_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04309354

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