Trifluoroacetic acid → Benzo(b)pyrido(4,3,2-de)(1,7)phenanthrolin-8-one

HRID 1370328ノート

反応式

HRID 1370328 の反応式
FC(F)(F)C([NH:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[C:12]1[C:21]2[C:20](=O)[C:19]3[CH:23]=[CH:24][CH:25]=[N:26][C:18]=3[C:17](=[O:27])[C:16]=2[N:15]=[CH:14][CH:13]=1)=O.FC(F)(F)C(O)=O>C(Cl)Cl>[CH:11]1[C:6]2=[N:5][C:20]3[C:19]4[C:18]([C:17](=[O:27])[C:16]5[C:21]=3[C:12]([CH:13]=[CH:14][N:15]=5)=[C:7]2[CH:8]=[CH:9][CH:10]=1)=[N:26][CH:25]=[CH:24][CH:23]=4

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 9908770HCID 9908770、化合物

生成物 1

HCID 9860577Benzo(b)pyrido(4,3,2-de)(1,7)phenanthrolin-8-one

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

30 mg (0.0756 mmol) of the compound of Example 4 and 1 mL of trifluoroacetic acid in 2 mL of CH2Cl2 are refluxed for 3 hours. After evaporating off the solvent on a rotary evaporator, the residue is taken up in 2 mL of 1N NaOH and 2 mL of CHCl3 and the mixture is stirred overnight. After recovering the organic phase, the aqueous phase is extracted with CHCl3 (5 times 10 mL). After drying the organic phases over MgSO4 and evaporating off the solvent on a rotary evaporator, 17 mg of compound are obtained in the form of yellow-colored crystals.

後処理

  1. customAfter evaporating off the solvent
  2. customon a rotary evaporator
  3. customAfter recovering the organic phase
  4. extractionthe aqueous phase is extracted with CHCl3 (5 times 10 mL)
  5. dry with materialAfter drying the organic phases over MgSO4
  6. customevaporating off the solvent
  7. customon a rotary evaporator, 17 mg of compound
  8. customare obtained in the form of yellow-colored crystals

出典と根拠

ORDレコード
ord-d9a36d72de7c4d1eb2519f9c3d5a08af
出典データセット
uspto-grants-2003_06
特許番号
US06583150B1

反応ノート

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