Triethylamine → HCID 57750993, Verbindung

HRID 2283374Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2283374
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([F:10])=[CH:4][C:3]=1[S:11]([NH2:14])(=[O:13])=[O:12].[Cl:15][C:16]1[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][C:17]=1[S:23](Cl)(=[O:25])=[O:24].C(N(CC)CC)C>ClCCl>[Cl:15][C:16]1[C:21]([Cl:22])=[CH:20][CH:19]=[CH:18][C:17]=1[S:23]([NH:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([F:10])=[CH:4][C:3]=1[S:11](=[O:13])(=[O:12])[NH2:14])(=[O:25])=[O:24]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 27342222,3-Dichlorobenzene-1-sulfonyl chlorideHCID 57750966HCID 57750966, Verbindung

Produkt 1

HCID 57750993HCID 57750993, VerbindungAusbeute 6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

2-Amino-5-fluoro-4-methoxybenzenesulfonamide (200 mg, 0.91 mmol) and 2,3-dichlorobenzene-1-sulfonyl chloride (290 mg, 1.18 mmol) were dissolved in anhydrous dichloromethane (5 mL). Anhydrous triethylamine (0.290 mL, 2.09 mmol) was added and the reaction was stirred at room temperature for 48 hours under an inert atmosphere. The reaction was quenched using 2 M hydrochloric acid (20 mL) and was extracted with dichloromethane. The combined organic phase were washed with water, dried over magnesium sulfate and concentrated under vacuum. Purification by preparative HPLC gave 23 mg (6% yield) of the title compound.

Aufarbeitung

  1. customThe reaction was quenched
  2. extractionwas extracted with dichloromethane
  3. washThe combined organic phase were washed with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under vacuum
  6. customPurification by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-436855f3f48d4cf3a22ad9d96ab504ee
Quelldatensatz
uspto-grants-2015_09
Patentnummer
US09145380B2

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