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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
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HRID 1767043 반응식
[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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참가 물질

8

반응물 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

생성물 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
수율 29.3%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 6212Chloroform용매2회

실험 절차

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)+.

후처리

  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)

출처 및 근거

ORD 기록
ord-4c73c418584f40c9be1ca10a3a9edaad
출처 데이터셋
uspto-grants-2007_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07232832B2

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