Acetic Acid → 5-(2-Nitro-ethyl)-2-phenoxy-pyridine

HRID 1694245

반응식

HRID 1694245 반응식
[N+:1](/[CH:4]=[CH:5]/[C:6]1[CH:7]=[CH:8][C:9]([O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][CH:11]=1)([O-:3])=[O:2].C(O)(=O)C.[B-].[Na+].O>CS(C)=O>[N+:1]([CH2:4][CH2:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=2)=[N:10][CH:11]=1)([O-:3])=[O:2]

참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 22959485VertellusHCID 592552955-((E)-2-Nitro-vinyl)-2-phenoxy-pyridine

생성물 1

HCID 576263415-(2-Nitro-ethyl)-2-phenoxy-pyridine

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

To a solution of 5-((E)-2-nitro-vinyl)-2-phenoxy-pyridine described in Manufacturing Example 232-1-3 (5.97 g, 24.6 mmol) and acetic acid (3.2 mL) in dimethyl sulfoxide (52 mL) was added sodium borohydrate (1.4 g, 36.9 mmol), at room temperature while cooling appropriately. This mixture was stirred for 30 minutes at room temperature. This mixture was cooled appropriately, then, water was added, which was stirred for 30 minutes at room temperature. This mixture was liquid-separated, and the organic layer was separated. The organic layer was washed with water, dried over anhydrous magnesium sulfate, and then filtered. The filtrate was concentrated under a reduced pressure to obtain the title compound (5.72 g) as a crude product.

후처리

  1. temperatureThis mixture was cooled appropriately
  2. stirringwhich was stirred for 30 minutes at room temperature
  3. customThis mixture was liquid-separated
  4. customthe organic layer was separated
  5. washThe organic layer was washed with water
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-b2bf1258499d4b7a90fb5efd6c2d5814
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158657B2

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