3-(2H-tetrazol-5-yl)-2-(trifluoromethyl)pyridine → Trifluoromethylpyridine

HRID 42671노트

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HRID 42671 반응식
COC1C=C(C=C([N+]([O-])=O)C=1OC)C(Cl)=NC.N1NN=NC=1[C:23]1[C:24]([C:29]([F:32])([F:31])[F:30])=[N:25][CH:26]=[CH:27][CH:28]=1>N1C=CC=CC=1>[F:30][C:29]([F:32])([F:31])[C:24]1[CH:23]=[CH:28][CH:27]=[CH:26][N:25]=1

참가 물질

4

반응물 2

HCID 687044913-(2H-tetrazol-5-yl)-2-(trifluoromethyl)pyridineHCID 866431073,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride

생성물 1

HCID 136199Trifluoromethylpyridine

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
82.5 °C

실험 절차

3,4-Dimethoxy-N-methyl-5-nitro-benzimidoyl chloride (0.28 g, 1.08 mmol) was added to a stirred solution of 3-(2H-tetrazol-5-yl)-2-(trifluoromethyl)pyridine (0.215 g, 1 mmol) in dry pyridine (3 mL), preheated to 50° C. The resulting mixture was cautiously heated to 75-90° C. and maintained at this temperature until nitrogen evolution ceased. The mixture was then poured onto water (30 mL) and extracted with dichloromethane (25 mL). The organic phase was separated, dried over anhydrous magnesium sulphate, filtered and evaporated to dryness. The resulting residue was purified by chromatography to afford 345-(3,4-dimethoxy-5-nitrophenyl)-4-methyl-4H-1,2,4-triazol-3-yl)-2-(trifluoromethyl)pyridine, 0.241 g (59%).

후처리

  1. custompreheated to 50° C
  2. temperaturemaintained at this temperature until nitrogen evolution
  3. additionThe mixture was then poured onto water (30 mL)
  4. extractionextracted with dichloromethane (25 mL)
  5. customThe organic phase was separated
  6. dry with materialdried over anhydrous magnesium sulphate
  7. filtrationfiltered
  8. customevaporated to dryness
  9. customThe resulting residue was purified by chromatography

출처 및 근거

ORD 기록
ord-feb33ba7b6c44a69a0c8e6a462be7d36
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536203B2

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