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

HRID 1730726ノート

反応式

HRID 1730726 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c897f0c38b0f4aecaa7953b7178bd282
出典データセット
uspto-grants-1976_11
特許番号
US03993677

反応ノート

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