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Water → HCID 69057074, Verbindung

HRID 1437644
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1437644
Cl.[CH:2]([C@H:15]1[C@@H:20]([O:21][CH2:22][C:23]2[CH:28]=[C:27]([C:29]([F:32])([F:31])[F:30])[CH:26]=[C:25]([F:33])[CH:24]=2)[CH2:19][CH2:18][NH:17][CH2:16]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[CH3:34][S:35](Cl)(=[O:37])=[O:36].O>C1COCC1.CCN(CC)CC>[CH:2]([C@H:15]1[C@@H:20]([O:21][CH2:22][C:23]2[CH:28]=[C:27]([C:29]([F:32])([F:30])[F:31])[CH:26]=[C:25]([F:33])[CH:24]=2)[CH2:19][CH2:18][N:17]([S:35]([CH3:34])(=[O:37])=[O:36])[CH2:16]1)([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 962WaterHCID 31297Methanesulfonyl chlorideHCID 69059221HCID 69059221, Verbindung

Produkt 1

HCID 69057074HCID 69057074, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 8028TetrahydrofuranLösungsmittelHCID 8471
Triethylamine
Lösungsmittel

Versuchsvorschrift

To a solution of the compound (28.8 mg) obtained in Example 26 in THF (2.0 ml), Et3N (25.1 μl) was added, methylsulfonyl chloride (9.3 μl) was added at 0° C., and the reaction mixture was reacted at room temperature 24 hours. The reaction mixture was poured into water, and then the product was extracted with ethyl acetate. The organic layer was washed with an aqueous 10% citric acid solution and saturated brine, and dried, and the solvent was evaporated under reduced pressure, and then the residue was purified by preparative HPLC to obtain the title compound.

Aufarbeitung

  1. customthe reaction mixture was reacted at room temperature 24 hours
  2. extractionthe product was extracted with ethyl acetate
  3. washThe organic layer was washed with an aqueous 10% citric acid solution and saturated brine
  4. customdried
  5. customthe solvent was evaporated under reduced pressure
  6. customthe residue was purified by preparative HPLC

Quellen und Nachweise

ORD-Eintrag
ord-2f8305a2e91b420081e6bfde3c05fcaa
Quelldatensatz
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07622487B2

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