Hydrochloric Acid → HCID 178517505, 화합물

HRID 1880663노트

반응식

HRID 1880663 반응식
[F:1][C:2]1[N:7]=[C:6]([C:8]([NH2:10])=O)[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1.[C:15](N1C=CN=C1)(N1C=CN=C1)=[O:16].[N:27]12CCCN=C1CCCCC2.Cl.[OH2:39]>O1CCCC1>[F:1][C:2]1[N:7]=[C:6]([C:8]2[NH:27][O:39][C:15](=[O:16])[N:10]=2)[CH:5]=[C:4]([C:11]([F:14])([F:13])[F:12])[CH:3]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 682631,1'-CarbonyldiimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 86647327HCID 86647327, 화합물

생성물 1

HCID 178517505HCID 178517505, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To 5 ml of tetrahydrofuran were added 0.6 g of 6-fluoro-4-trifluoromethylpyridine-2-carboxamide=oxime and 0.61 g of 1,1′-carbonyldiimidazole, and the mixture was stirred at room temperature for 2 hours and 30 minutes. Thereafter, 0.57 g of 1,8-diazabicyclo[5,4,0]undec-7-ene was added, and the mixture was stirred for 9 hours. To the reaction solution were added water and 10% HCl, the resultant solution was extracted with ethyl acetate three times, and the organic layers were combinedmm, dried with anhydrous magnesium sulfate, and concentrated. The residue was subjected to silica gel column chromatography to obtain 0.5 g of 3-(6-fluoro-4-trifluoromethylpyridin-2-yl)-1,2,4-oxadiazol-5-one (present compound (49)).

후처리

  1. stirringthe mixture was stirred for 9 hours
  2. extractionthe resultant solution was extracted with ethyl acetate three times
  3. dry with materialdried with anhydrous magnesium sulfate
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-0ceb2f76703644adb05d0a392fe379b7
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08318776B2

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