O-Methylhydroxylamine → 1-Methoxy-3-(1,2,3,4-tetrahydro-4-oxo-1-naphthyl)urea

HRID 1730726노트

반응식

HRID 1730726 반응식
[CH3:1][O:2][NH2:3].C(N(CC)CC)C.[O:11]=[C:12]1[C:21]2[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=2)[CH:15]([N:22]=[C:23]=[O:24])[CH2:14][CH2:13]1>C(Cl)Cl>[CH3:1][O:2][NH:3][C:23]([NH:22][CH:15]1[C:16]2[C:21](=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:12](=[O:11])[CH2:13][CH2:14]1)=[O:24]

참가 물질

5

반응물 3

HCID 4113O-MethylhydroxylamineHCID 8471TriethylamineHCID 203516844-Isocyanato-3,4-dihydronaphthalen-1(2H)-one

생성물 1

HCID 203516951-Methoxy-3-(1,2,3,4-tetrahydro-4-oxo-1-naphthyl)urea

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

A mixture of N-methoxyamine (2.5 g), triethylamine (3.04 g) and dry methylene chloride (50 ml) is stirred at room temperature for 20 minutes under a nitrogen atmosphere. Then a solution of 1,2,3,4-tetrahydro-4-oxo-1-naphthyl isocyanate (5.62 g) in dry methylene chloride (50 ml) is added dropwise. After stirring at room temperature for 40 minutes, the reaction mixture is evaporated to dryness in vacuo and the solid residue washed with water (3 × 150 ml) to yield 6.1 g. title product, m.p. 148° to 151° C. Recrystallization from benzene affords crystals, m.p. 155° to 158° C.

후처리

  1. stirringAfter stirring at room temperature for 40 minutes
  2. customthe reaction mixture is evaporated to dryness in vacuo
  3. washthe solid residue washed with water (3 × 150 ml)
  4. customto yield 6.1 g

출처 및 근거

ORD 기록
ord-c897f0c38b0f4aecaa7953b7178bd282
출처 데이터셋
uspto-grants-1976_11
특허 번호
US03993677

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