Trifluoroacetic acid → 7-(piperidin-4-yloxy)-3,4-dihydro-2H-2,4a,5-triaza-fluoren-1-one

HRID 2105433노트

반응식

HRID 2105433 반응식
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([O:14][C:15]2[CH:27]=[C:26]3[C:18]([N:19]4[C:24](=[CH:25]3)[C:23](=[O:28])[NH:22][CH2:21][CH2:20]4)=[N:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH:8]1[CH2:9][CH2:10][CH:11]([O:14][C:15]2[CH:27]=[C:26]3[C:18]([N:19]4[C:24](=[CH:25]3)[C:23](=[O:28])[NH:22][CH2:21][CH2:20]4)=[N:17][CH:16]=2)[CH2:12][CH2:13]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 684647274-(1-Oxo-1,2,3,4-tetrahydro-2,4a,5-triaza-fluoren-7-yloxy)-piperidine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 684660687-(piperidin-4-yloxy)-3,4-dihydro-2H-2,4a,5-triaza-fluoren-1-one수율 42%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

The solution of 0.45 g (1.17 mmol) 4-(1-oxo-1,2,3,4-tetrahydro-2,4a,5-triaza-fluoren-7-yloxy)-piperidine-1-carboxylic acid tert-butyl ester in 10 mL dichloromethane was cooled to 0° C., 5 mL (7.4 g, 65.3 mmol) trifluoroacetic acid were added and the cooling bath was removed. After 1 h the volatile components were removed at a rotary evaporator, the residue was dissolved in dichloromethane and was washed with 1M aqueous sodium hydroxide solution and brine. The organic layer was dried over magnesium sulfate, filtered and evaporated to give 140 mg (42%) of the desired product as a white solid.

후처리

  1. customthe cooling bath was removed
  2. customAfter 1 h the volatile components were removed at a rotary evaporator
  3. dissolutionthe residue was dissolved in dichloromethane
  4. washwas washed with 1M aqueous sodium hydroxide solution and brine
  5. dry with materialThe organic layer was dried over magnesium sulfate
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-862d7e4371584fafa39842a5ffdfed59
출처 데이터셋
uspto-grants-2009_08
특허 번호
US07579351B2

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