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Trifluoroacetic acid → HCID 67449594, 화합물

HRID 2370073
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HRID 2370073 반응식
FC(F)(F)C(O)=O.[Cl:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[N:16]([CH2:32][CH2:33][NH:34]C(=O)OC(C)(C)C)[C:17]2[C:22]([N:23]=1)=[C:21]([N:24]1[CH2:29][CH2:28][N:27]([CH3:30])[CH2:26][CH2:25]1)[N:20]=[C:19]([CH3:31])[N:18]=2>ClCCl>[Cl:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[C:15]1[N:16]([CH2:32][CH2:33][NH2:34])[C:17]2[C:22]([N:23]=1)=[C:21]([N:24]1[CH2:25][CH2:26][N:27]([CH3:30])[CH2:28][CH2:29]1)[N:20]=[C:19]([CH3:31])[N:18]=2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 67448282HCID 67448282, 화합물

생성물 1

HCID 67449594HCID 67449594, 화합물수율 101.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Add trifluoroacetic acid (5 mL) to a solution of tert-butyl N-[2-[8-(2-chlorophenyl)-2-methyl-6-(4-methylpiperazin-1-yl)purin-9-yl]ethyl]carbamate (0.51 g, 0.001 mol) in dichloromethane (5 mL) at 0° C. Allow the reaction to warm to room temperature and stir for 2 h. Quench the reaction mixture with saturated aqueous sodium bicarbonate solution and then extract with dichloromethane. Dry the organic layer over anhydrous sodium sulfate, filter, and concentrate to give 2-[8-(2-chlorophenyl)-2-methyl-6-(4-methylpiperazin-1-yl)purin-9-yl]ethanamine (0.39 g). ES/MS m/z 386 (M+1).

후처리

  1. customthe reaction
  2. customQuench the reaction mixture with saturated aqueous sodium bicarbonate solution
  3. extractionextract with dichloromethane
  4. dry with materialDry the organic layer over anhydrous sodium sulfate
  5. filtrationfilter
  6. concentrationconcentrate

출처 및 근거

ORD 기록
ord-9901a2f4997549359ce104f168d72164
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08710063B2

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