Acetic Acid → HCID 59255233, 화합물

HRID 1693967노트

반응식

HRID 1693967 반응식
C(O)(=O)C.[N:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][C:12]2[CH:19]=[CH:18][C:15]([CH:16]=O)=[CH:14][CH:13]=2)[CH:6]=1.[N+:20]([CH3:23])([O-:22])=[O:21].C([O-])(=O)C.[NH4+]>C(OCC)(=O)C.O>[N+:20](/[CH:23]=[CH:16]/[C:15]1[CH:18]=[CH:19][C:12]([O:11][C:7]2[CH:6]=[N:5][CH:10]=[CH:9][CH:8]=2)=[CH:13][CH:14]=1)([O-:22])=[O:21]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 6375NitromethaneHCID 517165Ammonium AcetateHCID 46774194-(Pyridin-3-yloxy)benzaldehyde

생성물 1

HCID 59255233HCID 59255233, 화합물수율 96.8%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
110 °C

실험 절차

To an acetic acid (17.0 mL) solution of 4-(pyridine-3-yloxy)-benzaldehyde (1.70 g, 8.53 mmol) described in Manufacturing Example 76-1-1 were added nitromethane (2.60 g, 42.7 mmol) and ammonium acetate (1.32 g, 17.1 mmol) under nitrogen atmosphere, which was stirred for 3 hours at 110° C. Water and ethyl acetate were added to the reaction solution, and the organic layer was then extracted with ethyl acetate. The organic layer was washed with water and saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (2.00 g) as a crude product.

후처리

  1. extractionthe organic layer was then extracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationThe filtrate was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-1041f3d722dc4217ae2449a5a1ece0ee
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158657B2

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