O-Methylhydroxylamine hydrochloride → HCID 178449944、化合物

HRID 529878ノート

反応式

HRID 529878 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([NH:17][CH:18]([CH:20]([CH3:22])[CH3:21])[CH3:19])=[C:9]([C:12](=O)[CH2:13][CH2:14][CH3:15])[C:10]#[N:11].Cl.[O:24]([NH2:26])[CH3:25]>C(O)C.S(=O)(=O)(O)O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]([NH:17][CH:18]([CH:20]([CH3:22])[CH3:21])[CH3:19])=[C:9]([C:12](=[N:26][O:24][CH3:25])[CH2:13][CH2:14][CH3:15])[C:10]#[N:11]

参加物

5

反応物 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 69671260HCID 69671260、化合物

生成物 1

HCID 178449944HCID 178449944、化合物収率 51%

試薬・触媒・溶媒 2

HCID 1118Sulfuric Acid触媒HCID 702Ethanol溶媒

実験手順

To a solution of 2-{(2-chlorophenyl)[(3-methylbutan-2-yl)amino]methylene}-3-oxohexanenitrile (0.300 g, 0.919 mmol, 1 eq.) in ethanol (6 ml) were added methoxylamine hydrochloride (0.314 g, 3.67 mmol, 4 eq.) followed by 2 drops of concentrated sulfuric acid. The reaction was microwaved (150° C., 22000 s, fixed hold, high absorption) and the solvent evaporated. The residual oil was triturated in ethyl acetate and washed with sat. aq. solution of NaCl. After drying over MgSO4 and concentration under vacuum, the residual oil was subjected to preparative HPLC to give 2-{(2-chlorophenyl)[(3-methylbutan-2-yl)amino]methylene}-3-(methoxyimino)hexanenitrile (0.163 g, 49% yield).

後処理

  1. customThe reaction was microwaved
  2. custom(150° C., 22000 s, fixed hold, high absorption)
  3. customthe solvent evaporated
  4. customThe residual oil was triturated in ethyl acetate
  5. washwashed with sat. aq. solution of NaCl
  6. dry with materialAfter drying over MgSO4 and concentration under vacuum

出典と根拠

ORDレコード
ord-c8f24266dcee4947b05b3b1e49ae0161
出典データセット
uspto-grants-2016_05
特許番号
US09351489B2

反応ノート

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