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

HRID 1370328노트

반응식

HRID 1370328 반응식
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

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 9908770HCID 9908770, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d9a36d72de7c4d1eb2519f9c3d5a08af
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06583150B1

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