Trifluoroacetic acid → 4'-Isopropyl-5-methyl-biphenyl-2-carboxylic acid (4-piperazin-1-yl-phenyl)-amide

HRID 1267116노트

반응식

HRID 1267116 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([NH:20][C:21]([C:23]3[C:24]([C:30]4[CH:35]=[CH:34][C:33]([CH:36]([CH3:38])[CH3:37])=[CH:32][CH:31]=4)=[CH:25][C:26]([CH3:29])=[CH:27][CH:28]=3)=[O:22])=[CH:16][CH:15]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(Cl)Cl>[N:11]1([C:14]2[CH:15]=[CH:16][C:17]([NH:20][C:21]([C:23]3[C:24]([C:30]4[CH:31]=[CH:32][C:33]([CH:36]([CH3:38])[CH3:37])=[CH:34][CH:35]=4)=[CH:25][C:26]([CH3:29])=[CH:27][CH:28]=3)=[O:22])=[CH:18][CH:19]=2)[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 540547824-{4-[(4'-Isopropyl-5-methyl-biphenyl-2-carbonyl)-amino]-phenyl}piperazine-1-carboxylic Acid Tert-Butyl Ester

생성물 1

HCID 537730414'-Isopropyl-5-methyl-biphenyl-2-carboxylic acid (4-piperazin-1-yl-phenyl)-amide수율 93.2%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 4-{4-[(4′-isopropyl-5-methyl-biphenyl-2-carbonyl)-amino]-phenyl}-piperazine-1-carboxylic acid tert-butyl ester (4 g) in CH2Cl2 (20 mL) was added trifluoroacetic acid (15 mL) and the solution was stirred at room temperature for 16 hours. The mixture was then evaporated under reduced pressure and the residue was taken in water and basified with a 1N NaOH aqueous solution. The resulting precipitate was extracted with CH2Cl2 and the organic phase was washed with water, dried over Na2SO4 filtered and evaporated to give the title compound (3 g) as white crystals.

후처리

  1. customThe mixture was then evaporated under reduced pressure
  2. extractionThe resulting precipitate was extracted with CH2Cl2
  3. washthe organic phase was washed with water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated

출처 및 근거

ORD 기록
ord-490d6c6cf0684d928abb461dbcef81d2
출처 데이터셋
uspto-grants-2003_04
특허 번호
US06552022B1

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