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Phosphorus oxychloride → 2-Chloro-6-(trifluoromethyl)-3H-imidazo[4,5-B]pyridine

HRID 730824
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HRID 730824 반응식
[F:1][C:2]([F:14])([F:13])[C:3]1[CH:4]=[C:5]2[NH:11][C:10](=O)[NH:9][C:6]2=[N:7][CH:8]=1.O=P(Cl)(Cl)[Cl:17]>>[Cl:17][C:10]1[NH:11][C:5]2[C:6]([N:9]=1)=[N:7][CH:8]=[C:3]([C:2]([F:14])([F:13])[F:1])[CH:4]=2
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참가 물질

3

반응물 2

HCID 24813Phosphorus oxychlorideHCID 117153916-Trifluoromethyl-1,3-dihydro-imidazo[4,5-b]pyridin-2-one

생성물 1

HCID 116801682-Chloro-6-(trifluoromethyl)-3H-imidazo[4,5-B]pyridine

실험 절차

A solution of 6-trifluoromethyl-1,3-dihydro-imidazo[4,5-b]pyridin-2-one from step (c) above (161 mg, 0.789 mmol) in POCl3 (5 mL) was heated at 95° C. for 16 h. The reaction mixture was cooled to room temperature, the solvent was removed in vacuo and the resulting oily residue was purified by silica gel column chromatography, eluting with EtOAc/hexane (1:3) to give the title compound as a light-yellow solid. MS (ESI positive ion) m/z: 222 (M+1).

후처리

  1. customthe solvent was removed in vacuo
  2. customthe resulting oily residue was purified by silica gel column chromatography
  3. washeluting with EtOAc/hexane (1:3)

출처 및 근거

ORD 기록
ord-85827168ede349e38f1315c2197ad4c4
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07582761B2

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