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

HRID 506749ノート

反応式

HRID 506749 の反応式
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

参加物

4

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-992f7ee78c1f44cdb1a3218005c16743
出典データセット
uspto-grants-2010_08
特許番号
US07786109B2

反応ノート

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