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Hydrochloric Acid → 3-Oxo-3,4-dihydro-2h-benzo[1,4]thiazine-6-sulfonic acid {3-[4-(6-methoxy-[1,5]naphthyridin-4-yl)-[1,2,3]triazol-1-yl]-propyl}amide

HRID 1767043
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1767043
[CH3:1][O:2][C:3]1[N:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[C:6]2[C:13]1[N:14]=[N:15][N:16]([CH2:18][CH2:19][CH2:20][N:21]2C(=O)C3C(=CC=CC=3)C2=O)[CH:17]=1.O.NN.Cl.C(N(CC)CC)C.[O:43]=[C:44]1[NH:49][C:48]2[CH:50]=[C:51]([S:54](Cl)(=[O:56])=[O:55])[CH:52]=[CH:53][C:47]=2[S:46][CH2:45]1>C(O)C.C(Cl)(Cl)Cl>[CH3:1][O:2][C:3]1[N:4]=[C:5]2[C:10](=[CH:11][CH:12]=1)[N:9]=[CH:8][CH:7]=[C:6]2[C:13]1[N:14]=[N:15][N:16]([CH2:18][CH2:19][CH2:20][NH:21][S:54]([C:51]2[CH:52]=[CH:53][C:47]3[S:46][CH2:45][C:44](=[O:43])[NH:49][C:48]=3[CH:50]=2)(=[O:56])=[O:55])[CH:17]=1
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Komponenten

8

Edukt 5

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 24654Hydrazine hydrate (1:1)HCID 211131512-{3-[4-(6-Methoxy-[1,5]naphthyridin-4-yl)-[1,2,3]triazol-1-yl]-propyl)-isoindole-1,3-dioneHCID 218737563-oxo-3,4-dihydro-2H-1,4-benzothiazine-6-sulfonyl chloride

Produkt 1

HCID 9806409
3-Oxo-3,4-dihydro-2h-benzo[1,4]thiazine-6-sulfonic acid {3-[4-(6-methoxy-[1,5]naphthyridin-4-yl)-[1,2,3]triazol-1-yl]-propyl}amide
Ausbeute 29,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

To a suspension of 2-{3-[4-(6-Methoxy-[1,5]naphthyridin-4-yl)-[1,2,3]triazol-1-yl]-propyl)-isoindole-1,3-dione (180 mg, 0.43 mmole) in ethanol (3 mL) was added hydrazine hydrate (23 μL, 0.48 mmole) and the mixture was brought to reflux for 3 hours. After cooling 0.1 mL of 6N aqueous HCl was added to dissolve the product. The mixture was filtered and the filtrate was concentrated to dryness to afford the crude amine hydrochloride (85 mg). This material was suspended in chloroform (3 mL) and treated with triethylamine (0.18 mL, 1.3 mmole), followed by 3-oxo-3,4-dihydro-2H benzo[1,4]thiazine-6-sulfonyl chloride (100 mg, 0.4 mmole). After stirring 1 hour the mixture was diluted with chloroform, washed with saturated aqueous NaHCO3, dried (MgSO4), and chromatographed on silica (0–5% methanovchloroform) to provide the title compound as an off-white solid (60 mg, 27%). 1H NMR (400 MHz, DMSO-d6): 10.83 (br s, 1 H); 9.05 (s, 1 H); 8.84 (d, 1H); 8.37 (d, 1H); 8.29 (d, 1H); 7.85 (m, 1H); 7.46 (d, 1H); 7.24–7.42 (m, 3H); 4.60 (m, 2H); 4.17 (s, 3H); 3.53 (s, 2H); 2.80 (m, 2H); 2.14 (m, 2H). LC-MS (ES) m/e 512 (M+H)+.

Aufarbeitung

  1. temperatureto reflux for 3 hours
  2. additionwas added
  3. dissolutionto dissolve the product
  4. filtrationThe mixture was filtered
  5. concentrationthe filtrate was concentrated to dryness
  6. customto afford the crude amine hydrochloride (85 mg)
  7. washwashed with saturated aqueous NaHCO3
  8. dry with materialdried (MgSO4)
  9. customchromatographed on silica (0–5% methanovchloroform)

Quellen und Nachweise

ORD-Eintrag
ord-4c73c418584f40c9be1ca10a3a9edaad
Quelldatensatz
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07232832B2

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