O-Methylhydroxylamine hydrochloride → HCID 178449944, 화합물

HRID 529878노트

반응식

HRID 529878 반응식
[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]

참가 물질

5

반응물 2

HCID 521874O-Methylhydroxylamine hydrochlorideHCID 69671260HCID 69671260, 화합물

생성물 1

HCID 178449944HCID 178449944, 화합물수율 51%

시약·촉매·용매 2

HCID 1118Sulfuric Acid촉매HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-c8f24266dcee4947b05b3b1e49ae0161
출처 데이터셋
uspto-grants-2016_05
특허 번호
US09351489B2

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