HCID 53968692, Verbindung → [(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl ester

HRID 2289685Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2289685
C([Si](C)(C)[O:6][C:7]1[CH:12]=[C:11]([CH:13]([CH3:15])[CH3:14])[C:10]([O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]2[C:26]([CH:27]([CH3:29])[CH3:28])=[CH:25][C:24]([CH:30]([CH3:32])[CH3:31])=[CH:23][C:22]=2[CH:33]([CH3:35])[CH3:34])=[C:9]([CH:39]([CH3:41])[CH3:40])[CH:8]=1)(C)(C)C>C(#N)C>[OH:6][C:7]1[CH:8]=[C:9]([CH:39]([CH3:41])[CH3:40])[C:10]([O:16][S:17](=[O:38])(=[O:37])[NH:18][C:19](=[O:36])[CH2:20][C:21]2[C:22]([CH:33]([CH3:34])[CH3:35])=[CH:23][C:24]([CH:30]([CH3:31])[CH3:32])=[CH:25][C:26]=2[CH:27]([CH3:29])[CH3:28])=[C:11]([CH:13]([CH3:15])[CH3:14])[CH:12]=1

Komponenten

3

Edukt 1

HCID 53968692HCID 53968692, Verbindung

Produkt 1

HCID 10142635[(2,4,6-Triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl esterAusbeute 90,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

A solution of 15 mL concentrated HF in 150 mL acetonitrile was added dropwise to a solution of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 4-(tert-butyl-dimethyl-silanyloxy)-2,6-diisopropyl-phenyl ester (9.71 g, 15.4 mmol) in 400 mL acetonitrile at room temperature under a nitrogen atmosphere. Stirred for 16 hours and then concentrated in vacuo. The residue was partitioned between water and dichloromethane. The organic layer was dried over magnesium sulfate, filtered, and concentrated to give an oily solid. Trituration with hexanes gave 7.24 g of [(2,4,6-triisopropyl-phenyl)-acetyl]-sulfamic acid 4-hydroxy-2,6-diisopropyl-phenyl ester as a white solid; mp 182-183° C.

Aufarbeitung

  1. concentrationA solution of 15 mL concentrated HF in 150 mL acetonitrile
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between water and dichloromethane
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customto give an oily solid

Quellen und Nachweise

ORD-Eintrag
ord-73bad4f621a34a42aa125a6923d52264
Quelldatensatz
uspto-grants-2000_07
Patentnummer
US06093744

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