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Phosphorus oxychloride → HCID 117974229, 화합물

HRID 2272923
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HRID 2272923 반응식
[CH3:1][N:2]1[C:6]2=[N:7][CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=[C:5]2[NH:4][C:3]1=O.P(Cl)(Cl)([Cl:18])=O.C(=O)(O)[O-].[Na+]>CN(C)C=O>[Cl:18][C:3]1[N:2]([CH3:1])[C:6]2=[N:7][CH:8]=[C:9]([C:11]([F:14])([F:13])[F:12])[CH:10]=[C:5]2[N:4]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 24813Phosphorus oxychlorideHCID 516892Sodium BicarbonateHCID 117974232HCID 117974232, 화합물

생성물 1

HCID 117974229HCID 117974229, 화합물수율 51.6%

시약·촉매·용매 1

HCID 6228Dimethylformamide촉매

반응 조건

온도
100 °C

실험 절차

A mixture of 1.09 g of 3-methyl-6-trifluoromethyl-1,3-dihydro-imidazo[4,5-b]pyridin-2-one, one drop of dimethylformamide and 10 g of phosphorus oxychloride was stirred at 100° C. for 3 hours. The cooled reaction mixture was poured to a saturated aqueous sodium bicarbonate solution, and the mixture was extracted twice with ethyl acetate. The combined organic layers were dried over anhydrous sodium sulfate and then concentrated under reduced pressure. The resulting residue was applied to a silica gel column chromatography to obtain 0.61 g of 2-chloro-3-methyl-6-trifluoromethyl-3H-imidazo[4,5-b]pyridine.

후처리

  1. customThe cooled reaction mixture
  2. extractionthe mixture was extracted twice with ethyl acetate
  3. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-3aff0ac0f0ba45ef8d77e4f556130336
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09120792B2

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