Lawesson's reagent → 2-(Tert-butyldiphenylsilyloxy)propanethioamide

HRID 872858

Reaktionsgleichung

Reaktionsgleichung von HRID 872858
COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:10]2)=CC=1.[Si:23]([O:40][CH:41]([CH3:45])[C:42]([NH2:44])=O)([C:36]([CH3:39])([CH3:38])[CH3:37])([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C1COCC1>[Si:23]([O:40][CH:41]([CH3:45])[C:42](=[S:10])[NH2:44])([C:36]([CH3:39])([CH3:38])[CH3:37])([C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

Komponenten

4

Edukt 2

HCID 87949Lawesson's reagentHCID 671685282-(Tertbutyldiphenylsilyloxy)propanamide

Produkt 1

HCID 872949642-(Tert-butyldiphenylsilyloxy)propanethioamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

A flask containing 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (387 mg, 0.957 mmol) was put under nitrogen atmosphere. 2-(tert-butyldiphenylsilyloxy)propanamide (622 mg, 1.899 mmol) dissolved in dry THF (10 ml) was added, temperature was raised to 60° C. and the mixture was allowed to react for 3 h. The solvent was evaporated and the product was extracted from DCM/water. The product was used in the next step without further purification. LC-MS: [M+1]=344.56.

Aufarbeitung

  1. additionwas added
  2. customto react for 3 h
  3. customThe solvent was evaporated
  4. extractionthe product was extracted from DCM/water
  5. customThe product was used in the next step without further purification

Quellen und Nachweise

ORD-Eintrag
ord-55ce6e08d68e4ee2846797447671d860
Quelldatensatz
uspto-grants-2015_03
Patentnummer
US08975254B2

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