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Hydrochloric Acid → (S)-tert-butyl 3-(((4-amino-2,2-dioxido-1H-benzo[c][1,2,6]thiadiazin-5-yl)oxy)methyl)piperidine-1-carboxylate

HRID 1483936
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1483936
[NH2:1][C:2]1[C:3]([C:23]#[N:24])=[C:4]([CH:20]=[CH:21][CH:22]=1)[O:5][CH2:6][C@H:7]1[CH2:12][CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:8]1.N1C=CC=CC=1.[S:31](Cl)(=[O:34])(=[O:33])[NH2:32].C([O-])(O)=O.[Na+].[OH-].[Na+].Cl>CC(N(C)C)=O.CCO.O>[NH2:24][C:23]1[C:3]2[C:4]([O:5][CH2:6][C@H:7]3[CH2:12][CH2:11][CH2:10][N:9]([C:13]([O:15][C:16]([CH3:19])([CH3:17])[CH3:18])=[O:14])[CH2:8]3)=[CH:20][CH:21]=[CH:22][C:2]=2[NH:1][S:31](=[O:34])(=[O:33])[N:32]=1
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Komponenten

10

Edukt 6

HCID 313Hydrochloric AcidHCID 1049PyridineHCID 14798Sodium HydroxideHCID 24499Chlorosulfamic acidHCID 516892Sodium BicarbonateHCID 86714276(S)-tert-butyl 3-((3-amino-2-cyanophenoxy)methyl)piperidine-1-carboxylate

Produkt 1

HCID 86714275
(S)-tert-butyl 3-(((4-amino-2,2-dioxido-1H-benzo[c][1,2,6]thiadiazin-5-yl)oxy)methyl)piperidine-1-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittelHCID 31374DimethylacetamideLösungsmittel

Versuchsvorschrift

To a solution of (S)-tert-butyl 3-((3-amino-2-cyanophenoxy)methyl)piperidine-1-carboxylate (Example 2c, 11.0 g, 33.2 mmol) in DMA (100 mL) was added pyridine (13.4 mL, 166 mmol) and sulfamoyl chloride (7.64 g, 66.4 mmol) in small portions. The mixture was stirred at room temperature under nitrogen for 1 hour until the reaction was complete according to LCMS. Saturated NaHCO3 was added until the mixture was neutral and the solution was extracted with EtOAc (3×). The combined organics were dried over Na2SO4 and concentrated. The residue was diluted with EtOH (100 mL) and NaOH (66.4 mL, 132.8 mmol, 2M solution) was added and the solution was heated to 80° C. for 3 hours. The reaction mixture was then allowed to cool to room temperature. The solution was further cool to 0° C. and neutralized with 2N HCl. Water was added and the desired product crashed out. The product was then filtered off and dried to yield the title compound (7.0 g, 51.4%). (M+H)−Boc=311.

Aufarbeitung

  1. extractionthe solution was extracted with EtOAc (3×)
  2. dry with materialThe combined organics were dried over Na2SO4
  3. concentrationconcentrated
  4. additionwas added
  5. temperaturethe solution was heated to 80° C. for 3 hours
  6. temperatureto cool to room temperature

Quellen und Nachweise

ORD-Eintrag
ord-c8e728409e9a42348d16a3d1b9ba4037
Quelldatensatz
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09420814B2

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