HCID 68585893, 화합물 → 7-fluoro-5-methyl-2-[methyl(1H-1,2,4-triazol-5-ylmethyl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile

HRID 17433노트

반응식

HRID 17433 반응식
[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:4]([CH3:30])[C:5]([C:28]#[N:29])=[C:6]2[C:10]=1[O:9][C:8]([N:11]([CH3:27])[CH2:12][C:13]1[N:14](CC3C=CC(OC)=CC=3)[N:15]=[CH:16][N:17]=1)=[N:7]2>FC(F)(F)C(O)=O>[F:1][C:2]1[C:3]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)=[C:4]([CH3:30])[C:5]([C:28]#[N:29])=[C:6]2[C:10]=1[O:9][C:8]([N:11]([CH3:27])[CH2:12][C:13]1[NH:14][N:15]=[CH:16][N:17]=1)=[N:7]2

참가 물질

3

반응물 1

HCID 68585893HCID 68585893, 화합물

생성물 1

HCID 685848557-fluoro-5-methyl-2-[methyl(1H-1,2,4-triazol-5-ylmethyl)amino]-6-phenyl-1,3-benzoxazole-4-carbonitrile수율 97.4%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

7-Fluoro-2-[N-[[2-(4-methoxybenzyl)-2-H-[1,2,4]triazol-3-yl]methyl]methylamino]-5-methyl-6-phenyl-1,3-benzoxazole-4-carbonitrile (I-164) (0.33 g, 0.68 mmol) was dissolved in trifluoroacetic acid (5 ml), and stirred at room temperature for 16 hours, then at an external temperature of about 60° C. for 6 hours. The solvent was evaporated away under reduced pressure, then ethyl acetate and aqueous sodium hydrogencarbonate solution were added, and the organic layer was separated. After drying over anhydrous sodium sulfate, the solvent was evaporated away under reduced pressure, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1) to obtain a colorless solid (0.24 g, 97%).

후처리

  1. waitat an external temperature of about 60° C. for 6 hours
  2. customThe solvent was evaporated away under reduced pressure
  3. additionethyl acetate and aqueous sodium hydrogencarbonate solution were added
  4. customthe organic layer was separated
  5. dry with materialAfter drying over anhydrous sodium sulfate
  6. customthe solvent was evaporated away under reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=20:1)

출처 및 근거

ORD 기록
ord-63d3818bb09c4d659eede15646fa4e51
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737166B2

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