6-Chloro-3-methyl-1-propyl-2,4(1H,3H)-pyrimidinedione → 6-Mercapto-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione

HRID 131561

Reaktionsgleichung

Reaktionsgleichung von HRID 131561
Cl[C:2]1[N:7]([CH2:8][CH2:9][CH3:10])[C:6](=[O:11])[N:5]([CH3:12])[C:4](=[O:13])[CH:3]=1.O.[SH-:15].[Na+]>C(O)C>[SH:15][C:2]1[N:7]([CH2:8][CH2:9][CH3:10])[C:6](=[O:11])[N:5]([CH3:12])[C:4](=[O:13])[CH:3]=1

Komponenten

4

Edukt 2

HCID 8169336-Chloro-3-methyl-1-propyl-2,4(1H,3H)-pyrimidinedioneHCID 16211346Sodium hydrosulfide hydrate

Produkt 1

HCID 866227106-Mercapto-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A mixture of 6-chloro-3-methyl-1-propyl-pyrimidine-2,4(1H,3H)-dione (3.76 g), sodium hydrosulphide hydrate (6 g) and ethanol (100 ml) was stirred at room temperature for 48 hours then concentrated in vacuo. The residue was dissolved in water (500 ml) and washed with ethyl acetate (2×100 ml). The aqueous phase was acidified with dilute hydrochloric acid, then extracted with ethyl acetate (3×100 ml). The combined organic phase was dried (MgSO4) and evaporated to leave a pale yellow solid which was used directly in the next step.

Aufarbeitung

  1. concentrationthen concentrated in vacuo
  2. dissolutionThe residue was dissolved in water (500 ml)
  3. washwashed with ethyl acetate (2×100 ml)
  4. extractionextracted with ethyl acetate (3×100 ml)
  5. dry with materialThe combined organic phase was dried (MgSO4)
  6. customevaporated
  7. customto leave a pale yellow solid which

Quellen und Nachweise

ORD-Eintrag
ord-aa2686d9fed644a8b4ea57c0b60b8015
Quelldatensatz
uspto-grants-2008_06
Patentnummer
US07384950B2

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