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

HRID 640575노트

반응식

HRID 640575 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-2e0e58aa494f4ace9d2da5ce3e9b1a39
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07691882B2

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