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Trifluoroacetic acid → N-(5-benzenesulfonyl-1H-indazol-3-yl)-4-(4-methyl-piperazin-1-yl)-2-(tetrahydro-pyran-4-ylamino)-benzamide

HRID 1640983
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HRID 1640983 반응식
[NH2:1][C:2]1[CH:28]=[C:27]([N:29]2[CH2:34][CH2:33][N:32]([CH3:35])[CH2:31][CH2:30]2)[CH:26]=[CH:25][C:3]=1[C:4]([NH:6][C:7]1[C:15]2[C:10](=[CH:11][CH:12]=[C:13]([S:16]([C:19]3[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=3)(=[O:18])=[O:17])[CH:14]=2)[NH:9][N:8]=1)=[O:5].FC(F)(F)C(O)=O.[O:43]1[CH2:48][CH2:47][C:46](=O)[CH2:45][CH2:44]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.C[N+](C)(C)C.[H-]>ClCCl>[C:19]1([S:16]([C:13]2[CH:14]=[C:15]3[C:10](=[CH:11][CH:12]=2)[NH:9][N:8]=[C:7]3[NH:6][C:4](=[O:5])[C:3]2[CH:25]=[CH:26][C:27]([N:29]3[CH2:30][CH2:31][N:32]([CH3:35])[CH2:33][CH2:34]3)=[CH:28][C:2]=2[NH:1][CH:46]2[CH2:47][CH2:48][O:43][CH2:44][CH2:45]2)(=[O:18])=[O:17])[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1
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참가 물질

7

반응물 5

HCID 6422Trifluoroacetic acidHCID 121599Tetrahydro-4H-pyran-4-oneHCID 166653HydrideHCID 13696215Tetramethylammonium Triacetoxyborohydride (>90%)HCID 594370872-amino-N-(5-benzenesulfonyl-1H-indazol-3-yl)-4-(4-methyl-piperazin-1-yl)-benzamide

생성물 1

HCID 59437048
N-(5-benzenesulfonyl-1H-indazol-3-yl)-4-(4-methyl-piperazin-1-yl)-2-(tetrahydro-pyran-4-ylamino)-benzamide
수율 64.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

2-Amino-N-(5-benzenesulfonyl-1H-indazol-3-yl)-4-(4-methyl-piperazin-1-yl)-benzamide (245 mg, 0.5 mmol) was dissolved in dichloromethane (5 mL) and trifluoroacetic acid (0.77 mL, 10 mmol), treated first with tetrahydro-pyran-4-one (0.055 mL, 0.6 mmol) and then with tetramethylammonium triacetoxyborohydride (197 mg, 0.75 mmol). The reaction was stirred at room temperature overnight then additional ketone (0.055 mL, 0.6 mmol) and hydride (2 portions: 197 mg first and 50 mg after a couple of hours) were added. After additional stirring overnight the volatiles were removed under reduced pressure. Dichloromethane was added and the organic phase was washed with aqueous sodium hydrogen carbonate, dried over sodium sulfate and evaporated. The crude product was purified by flash chromatography over silica gel (eluent: dichloromethane/methanol/33% NH4OH in 95:5:1 ratio) affording 186 mg of product still containing some impurities. Further purification by preparative HPLC (basic method) gave 80 mg of title compound.

후처리

  1. stirringAfter additional stirring overnight the volatiles
  2. customwere removed under reduced pressure
  3. additionDichloromethane was added
  4. washthe organic phase was washed with aqueous sodium hydrogen carbonate
  5. dry with materialdried over sodium sulfate
  6. customevaporated
  7. customThe crude product was purified by flash chromatography over silica gel (eluent: dichloromethane/methanol/33% NH4OH in 95:5:1 ratio)

출처 및 근거

ORD 기록
ord-ca6f13613b53443193399985d485bd48
출처 데이터셋
uspto-grants-2012_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08114865B2

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