Trifluoroacetic acid → HCID 178434437, 화합물

HRID 1629952노트

반응식

HRID 1629952 반응식
COC1C=CC(C[N:8]2[C:12]3=[N:13][CH:14]=[C:15]([C:17]4[CH:22]=[CH:21][C:20]([N:23]5[CH2:28][CH2:27][N:26]([CH3:29])[CH2:25][CH2:24]5)=[CH:19][CH:18]=4)[CH:16]=[C:11]3[C:10]([CH3:30])=[N:9]2)=CC=1.FC(F)(F)C(O)=O>C(Cl)(Cl)Cl>[CH3:30][C:10]1[C:11]2[C:12](=[N:13][CH:14]=[C:15]([C:17]3[CH:18]=[CH:19][C:20]([N:23]4[CH2:24][CH2:25][N:26]([CH3:29])[CH2:27][CH2:28]4)=[CH:21][CH:22]=3)[CH:16]=2)[NH:8][N:9]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 683884351-(4-methoxybenzyl)-3-methyl-5-(4-(4-methylpiperazin-1-yl)phenyl)-1H-pyrazolo[3,4-b]pyridine

생성물 1

HCID 178434437HCID 178434437, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
50 °C

실험 절차

To a stirred solution of 1-(4-methoxybenzyl)-3-methyl-5-(4-(4-methylpiperazin-1-yl)phenyl)-1H-pyrazolo[3,4-b]pyridine (160) in CHCl3 (20 mL) was added trifluoroacetic acid (5 mL) and heated at 50° C. for 12 hours. After completion of the reaction the solvents were removed, diluted with cold water, pH was adjusted to 8 and the aqueous phase extracted with chloroform twice. The organic layer was washed with brine solution and dried over sodium sulphate and the solvent completely distilled off to get the crude product. The crude was passed through 100-200 mesh silica gel, eluting the pure compound in 10% MeOH/CHCl3 as pale yellow solid compound 161 (8 mg).

후처리

  1. customAfter completion of the reaction the solvents
  2. customwere removed
  3. additiondiluted with cold water, pH
  4. extractionthe aqueous phase extracted with chloroform twice
  5. washThe organic layer was washed with brine solution
  6. dry with materialdried over sodium sulphate
  7. distillationthe solvent completely distilled off

출처 및 근거

ORD 기록
ord-ef5b9f228f244d42a6692d48cb203429
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791112B2

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