Piperidinium acetate → HCID 178456894, 화합물

HRID 1620636노트

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HRID 1620636 반응식
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:19]=[C:18]([C:20]([F:23])([F:22])[F:21])[CH:17]=[CH:16][C:4]=1[CH2:5][N:6]1[C:12](=[O:13])[CH2:11][CH2:10][CH:9]([CH:14]=O)[CH2:8][CH2:7]1.[CH2:26]([NH:29][C:30]1[CH2:34][S:33][C:32](=[O:35])[N:31]=1)[C:27]#[CH:28].C([O-])(=O)C.[NH2+]1CCCCC1>CC(O)C>[F:24][C:2]([F:25])([F:1])[C:3]1[CH:19]=[C:18]([C:20]([F:23])([F:21])[F:22])[CH:17]=[CH:16][C:4]=1[CH2:5][N:6]1[CH2:7][CH2:8][CH:9](/[CH:14]=[C:34]2/[C:30]([NH:29][CH2:26][C:27]#[CH:28])=[N:31][C:32](=[O:35])[S:33]/2)[CH2:10][CH2:11][C:12]1=[O:13]

참가 물질

5

반응물 3

HCID 3014295Piperidinium acetateHCID 866788021-[2,4-Bis(trifluoromethyl)benzyl]-7-oxoazepane-4-carbaldehydeHCID 178456890HCID 178456890, 화합물

생성물 1

HCID 178456894HCID 178456894, 화합물수율 35%

시약·촉매·용매 1

HCID 3776Isopropanol용매

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온도
80 °C

실험 절차

To a solution of 1-[2,4-bis(trifluoromethyl)benzyl]-7-oxoazepane-4-carbaldehyde (1.00 g) and 4-(prop-2-yn-1-ylamino)-1,3-thiazol-2(5H)-one (0.63 g) in 2-propanol (10 mL) was added piperidinium acetate (0.40 g). The reaction mixture was stirred at 80° C. for 2 hr and concentrated. Water was added to the residue, and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (0.48 g).

후처리

  1. concentrationconcentrated
  2. additionWater was added to the residue
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe extract was washed with saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customthe solvent was evaporated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-410c56fd6be14151b571ba61869b5d67
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772277B2

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