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Hydrogen Peroxide → HCID 178476844, 화합물

HRID 482443
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HRID 482443 반응식
[C:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10]([C:12]1[CH:26]=[CH:25][C:15]([CH2:16][P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])=[CH:14][CH:13]=1)=O)#[N:2].[OH:27]O.[OH-].[Na+]>C1COCC1.[Cl-].[Na+].O>[OH:27][C:1]1[C:3]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:9]=[C:10]([C:12]2[CH:26]=[CH:25][C:15]([CH2:16][P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20])=[CH:14][CH:13]=2)[N:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 784Hydrogen PeroxideHCID 14798Sodium HydroxideHCID 10738021diethyl 4-[N-(2-cyanophenyl)carbamoyl]benzylphosphonate

생성물 1

HCID 178476844HCID 178476844, 화합물

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매HCID 57417360Sodium chloride; water용매

실험 절차

Diethyl 4-[N-(2-cyanophenyl)carbamoyl]benzylphosphonate (11.2 g) was dissolved in 100 ml of THF and cooled with ice water. After adding 50 ml of a 30% hydrogen peroxide aqueous solution containing 1.2 g of sodium hydroxide dropwise, the reaction mixture was stirred at room temperature for 16 hours. Saturated brine (50 ml) was added, and the reaction mixture was extracted with chloroform. The chloroform layer was dried over magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was dissolved in 150 ml of ethanol and 20 ml of a 2N sodium hydroxide solution and stirred at room temperature for 6 hours. Saturated brine (150 ml) was added, and the reaction mixture was extracted with chloroform. The chloroform layer was dried over magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was recrystallized with methylene chloride-diethyl ether to give 5.9 g of diethyl 4-(4-hydroxyquinazolin-2-yl)benzylphosphonate as colorless crystals.

후처리

  1. extractionthe reaction mixture was extracted with chloroform
  2. dry with materialThe chloroform layer was dried over magnesium sulfate
  3. distillationthe solvent was distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in 150 ml of ethanol
  5. stirring20 ml of a 2N sodium hydroxide solution and stirred at room temperature for 6 hours
  6. additionSaturated brine (150 ml) was added
  7. extractionthe reaction mixture was extracted with chloroform
  8. dry with materialThe chloroform layer was dried over magnesium sulfate
  9. distillationthe solvent was distilled off under reduced pressure
  10. customThe residue was recrystallized with methylene chloride-diethyl ether

출처 및 근거

ORD 기록
ord-d5568d12ef1242a6b07d99407bf7fd13
출처 데이터셋
uspto-grants-1998_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05798344

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