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Sodium Hypochlorite → 2-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamate

HRID 551723
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HRID 551723 반응식
[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]([NH:8][NH:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])=[O:7].Cl[O-].[Na+]>C1(C)C=CC=CC=1>[CH3:1][O:2][CH2:3][CH2:4][O:5][C:6]([N:8]=[N:9][C:10]([O:12][CH2:13][CH2:14][O:15][CH3:16])=[O:11])=[O:7]
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참가 물질

4

반응물 2

HCID 23665760Sodium HypochloriteHCID 249880741,2-Bis(2-methoxyethyl) 1,2-hydrazinedicarboxylate

생성물 1

HCID 533844152-methoxyethyl N-(2-methoxyethoxycarbonylimino)carbamate수율 37%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

To a solution obtained by adding 1,2-hydrazinedicarboxylic acid bis(2-methoxyethyl) ester (200 mg, 0.85 mmol) and toluene (2 mL) to a 10 mL flask, followed by cooling with an ice bath, was added dropwise a 5% sodium hypochlorite solution (1.39 g, 0.85 mmol), and the reaction was allowed to proceed for one hour. After the reaction, the solution was washed with water (1 mL, ×2), and dehumidified with anhydrous magnesium sulfate, followed by concentration to dryness. The resulting solid was recrystallized with toluene (1 mL) and hexane (5 mL), to give azodicarboxylic acid bis(2-methoxyethyl) ester as a pale yellow crystal (73 mg, yield: 37%).

후처리

  1. customTo a solution obtained
  2. temperatureby cooling with an ice bath
  3. customAfter the reaction
  4. washthe solution was washed with water (1 mL, ×2)
  5. concentrationfollowed by concentration to dryness
  6. customThe resulting solid was recrystallized with toluene (1 mL) and hexane (5 mL)

출처 및 근거

ORD 기록
ord-26f20dc7d4574b2ba5fcb028ba9e9038
출처 데이터셋
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07947816B2

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