Benzoyl chloride → HCID 178520224, Verbindung
Reaktionsgleichung
O1CCCCC1[N:7]1[C:15]2[C:10](=[CH:11][C:12]([C:16]3[N:20]=[CH:19][N:18](C(C4C=CC=CC=4)(C4C=CC=CC=4)C4C=CC=CC=4)[N:17]=3)=[CH:13][CH:14]=2)[C:9]([C:40]2[CH:45]=[CH:44][C:43]([NH2:46])=[CH:42][CH:41]=2)=[N:8]1.[C:47](Cl)(=O)[C:48]1C=CC=[CH:50][CH:49]=1.C(N(CC)CC)C.[O:63]1[CH2:67][CH2:66][CH2:65][CH2:64]1>>[NH:18]1[CH:19]=[N:20][C:16]([C:12]2[CH:11]=[C:10]3[C:15](=[CH:14][CH:13]=2)[NH:7][N:8]=[C:9]3[C:40]2[CH:45]=[CH:44][C:43]([NH:46][C:67](=[O:63])[CH2:66][C:65]3[CH:50]=[CH:49][CH:48]=[CH:47][CH:64]=3)=[CH:42][CH:41]=2)=[N:17]1Komponenten
5
Versuchsvorschrift
The title compound was prepared as described in Example 376, using 4-{1-perhydro-2H-pyran-2-yl-5-[1-(triphenylmethyl)(1,2,4-triazol-3-yl)]-1H-indazol-3-yl}phenylamine (0.303 g, 0.50 mmol) in tetrahydrofuran (4.5 mL) was added benzoyl chloride (0.10 mL, 0.76 mmol) and triethylamine (0.35 mL, 2.52 mmol). The final crude product was purified by preparative HPLC (30–80% acetonitrile to H2O, 30 min.) (0.010 g, 5% yield): 1H NMR (DMSO-d6) δ 10.37 (s, 1H), 8.68 (br s, 1H), 8.07 (d, 1H), 7.95 (br s, 2H), 7.80 (d, 2H), 7.69 (br s, 1H), 7.30 (m, 5H), 3.69 (s, 2H); ES-MS (m/z) 395 [M+1]+.
Aufarbeitung
- customThe final crude product was purified by preparative HPLC (30–80% acetonitrile to H2O, 30 min.) (0.010 g, 5% yield)
Quellen und Nachweise
- ORD-Eintrag
- ord-58c0a6f9f4b041c9ac83a4c38c5195ca
- Quelldatensatz
- uspto-grants-2007_04
- Patentnummer
- US07208513B2
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