1,1'-Carbonyldiimidazole → HCID 59683283, 화합물

HRID 447778노트

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HRID 447778 반응식
[NH2:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH:9]2[CH2:11][CH2:10]2)=[CH:4][C:3]=1[NH:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]1.C1N=CN([C:31](N2C=NC=C2)=[O:32])C=1>O1CCCC1>[CH:9]1([C:5]2[CH:6]=[C:7]([F:8])[C:2]3[NH:1][C:31](=[O:32])[N:12]([CH:13]4[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]4)[C:3]=3[CH:4]=2)[CH2:11][CH2:10]1

참가 물질

4

반응물 2

HCID 682631,1'-Carbonyldiimidazole2회HCID 596832651,1-Dimethylethyl 4-[(2-amino-5-cyclopropyl-3-fluorophenyl)amino]-1-piperidinecarboxylate

생성물 1

HCID 59683283HCID 59683283, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

1,1-Dimethylethyl 4-[(2-amino-5-cyclopropyl-3-fluorophenyl)amino]-1-piperidine-carboxylate (D27, 0.80 mmol, 280 mg) was dissolved in 4 ml of tetrahydrofuran and CDI (1,1′-(oxomethanediyl)bis-1H-imidazole) (2.5 eq., 2.0 mmol, 0.33 g) at room temperature and the mixture was stirred at 50° C. for one overnight under argon. Extra CDI (1 eq., 0.13 g, 0.80 mmol) was added and the mixture was refluxed for two extra hours. The mixture was cooled to room temperature and the solvent was evaporated to afford the crude compound which was purified by chromatography (ethyl acetate (50)-n-hexane (50)) to yield the title compound, 102 mg, 36%, M−−H=374.

후처리

  1. temperaturethe mixture was refluxed for two extra hours
  2. customthe solvent was evaporated
  3. customto afford the crude compound which
  4. customwas purified by chromatography (ethyl acetate (50)-n-hexane (50))

출처 및 근거

ORD 기록
ord-31e4022220ac4886b885c3cebeea2491
출처 데이터셋
uspto-grants-2013_07
특허 번호
US08481566B2

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