S,S-dimethyl carbonodithioate → 5-Triisopropylsilanyloxy-tetrahydro-pyrimidin-2-one

HRID 2204324

Reaktionsgleichung

Reaktionsgleichung von HRID 2204324
[CH:1]([Si:4]([CH:14]([CH3:16])[CH3:15])([CH:11]([CH3:13])[CH3:12])[O:5][CH:6]([CH2:9][NH2:10])[CH2:7][NH2:8])([CH3:3])[CH3:2].[C:17](SC)(=[O:20])SC>CO>[CH:14]([Si:4]([CH:11]([CH3:13])[CH3:12])([CH:1]([CH3:3])[CH3:2])[O:5][CH:6]1[CH2:7][NH:8][C:17](=[O:20])[NH:10][CH2:9]1)([CH3:16])[CH3:15]

Komponenten

4

Edukt 2

HCID 313474S,S-dimethyl carbonodithioateHCID 867031322-Triisopropylsilanyloxy-propane-1,3-diamine

Produkt 1

HCID 867031315-Triisopropylsilanyloxy-tetrahydro-pyrimidin-2-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
60 °C

Versuchsvorschrift

To a solution of 2-triisopropylsilanyloxy-propane-1,3-diamine (Step P10) (27.8 g, 113 mmol) in MeOH (450 mL) was added S,S-dimethyl carbonodithioate (17.7 mL, 169 mmol) and the mixture was stirred at 60° C. for 20 h. The reaction mixture was concentrated. The residue was purified by flash chromatography(CH2Cl2/MeOH, 100:0→5:1) to afford the title compound. ESI-MS: [M+H]+273.3 (LC-MS 1-flow injection).

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated
  2. customThe residue was purified by flash chromatography(CH2Cl2/MeOH, 100:0→5:1)

Quellen und Nachweise

ORD-Eintrag
ord-81305d4da4ce403c979021e5597f44da
Quelldatensatz
uspto-grants-2016_06
Patentnummer
US09365576B2

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