1,2-Dichloroethane → HCID 59625331, 화합물

HRID 2192806노트

반응식

HRID 2192806 반응식
[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH:7][C:8]1[N:13]=[C:12]2[C:14]([CH3:18])([CH3:17])[CH2:15][CH2:16][C:11]2=[CH:10][C:9]=1[C:19]([OH:21])=O.CC(C)[CH2:24][NH:25][CH:26]1[CH2:31][CH2:30][CH2:29][N:28]([C:32]([O:34][C:35]([CH3:38])([CH3:37])[CH3:36])=[O:33])[CH2:27]1.[CH:40](N(CC)C(C)C)(C)C.F[P-](F)(F)(F)(F)F.ClC(N(C)C)=[N+](C)C.Cl[CH2:65][CH2:66]Cl>C(=O)([O-])O.[Na+]>[O:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][NH:7][C:8]1[N:13]=[C:12]2[C:14]([CH3:17])([CH3:18])[CH2:15][CH2:16][C:11]2=[CH:10][C:9]=1[C:19]([N:25]([CH2:24][CH:65]([CH3:66])[CH3:40])[CH:26]1[CH2:31][CH2:30][CH2:29][N:28]([C:32]([O:34][C:35]([CH3:37])([CH3:36])[CH3:38])=[O:33])[CH2:27]1)=[O:21]

참가 물질

7

반응물 5

HCID 111,2-DichloroethaneHCID 81531DiisopropylethylamineHCID 10989639Chloro-N,N,N',N'-tetramethylformamidinium HexafluorophosphateHCID 59625412HCID 59625412, 화합물HCID 59625616HCID 59625616, 화합물

생성물 1

HCID 59625331HCID 59625331, 화합물

시약·촉매·용매 1

HCID 516892Sodium Bicarbonate용매

실험 절차

2-[(Furan-2-ylmethyl)amino]-7,7-dimethyl-6,7-dihydro-5H-cyclopenta[b]pyridine-3-carboxylic acid (390 mg), tert-butyl 3-[(2-methylpropyl)amino]piperidine-1-carboxylate (350 mg) and N,N-diisopropylethylamine (1.2 ml) were dissolved in 1,2-dichloroethane (10 ml), chloro-N,N,N′,N′-tetramethylformamidinium hexafluorophosphate (540 mg) was added and the mixture was stirred at room temperature for 18 hr. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution and the mixture was extracted with ethyl acetate. The extract was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The residue was subjected to silica gel column chromatography, and the fraction eluted with ethyl acetate-hexane (5:95-100:10) was concentrated under reduced pressure to give the object compound (123 mg).

후처리

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe extract was washed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. washthe fraction eluted with ethyl acetate-hexane (5:95-100:10)
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-7900202318e4429485bd03378be85890
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329691B2

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