Sulfuric Acid → alpha-Oximino-3-pyridylacetonitrile

HRID 727361

반응식

HRID 727361 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][C:8]#[N:9])[CH:2]=1.[OH-].[Na+].C[O:13][N:14]=O.S(=O)(=O)(O)O.N([O-])=O.[Na+]>CO.O>[N:14](=[C:7]([C:3]1[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=1)[C:8]#[N:9])[OH:13]

참가 물질

8

반응물 5

HCID 1118Sulfuric AcidHCID 12231Methyl nitriteHCID 14798Sodium HydroxideHCID 809233-Pyridineacetonitrile2회HCID 23668193Sodium Nitrite

생성물 1

HCID 72747148alpha-Oximino-3-pyridylacetonitrile

시약·촉매·용매 2

HCID 887Methanol용매2회HCID 962Water용매2회

반응 조건

온도
0 °C

실험 절차

3-pyridylacetonitrile (47.2 g, 400 mmol) was dissolved in a solution of sodium hydroxide (16 g, 400 mmol) in methanol (100 ml). Methylnitrite, generated by dropping a solution of concentrated sulphuric acid (12.8 ml) and water (26 ml) to a solution of sodium nitrite (33.2 g, 480 mmol) in water (20 ml) and methanol (20 ml), was bobled through the 3-pyridylacetonitrile solution at 0° C. The reaction mixture was stirred at 0° C. for 1 h and the precipitate collected by filtration. The precipitate was washed with a little methanol to give the wanted product in 70% (41.1 g) yield. M+ : 147.

후처리

  1. filtrationthe precipitate collected by filtration
  2. washThe precipitate was washed with a little methanol
  3. customto give the wanted product in 70% (41.1 g)
  4. customyield

출처 및 근거

ORD 기록
ord-d523e78b3b704463bb832fb2d59a95bc
출처 데이터셋
uspto-grants-1998_01
특허 번호
US05712297

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