Water → HCID 131733986, Verbindung

HRID 712353Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 712353
Br.[C:2]([S:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=1)(=[NH:4])[NH2:3].[C:16]([O-])(=O)[CH3:17].[NH4+].C([N:23]=[C:24]=[O:25])C.O>CN(C=O)C>[CH2:16]([N:13]([CH2:10][CH3:11])[C:24]([NH2:23])=[O:25])[CH3:17].[N+:13]([C:10]1[CH:11]=[CH:12][C:7]([CH2:6][S:5][C:2](=[NH:3])[NH2:4])=[CH:8][CH:9]=1)([O-:15])=[O:14]

Komponenten

6

Edukt 4

HCID 962WaterHCID 8022Ethyl isocyanateHCID 116350Pseudourea, 2-(p-nitrobenzyl)-2-thio-, monohydrobromideHCID 517165Ammonium Acetate

Produkt 1

HCID 131733986HCID 131733986, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

To a solution of 4-nitrobenzyl carbamimidothioate hydrobromide (2.5 g, 8.55 mmol) in DMF (10 mL) was added aqueous buffer solution of ammonium acetate (pH ˜7, 4.0 mL) followed by addition of ethyl isocyanate (10 mL. 85.57 mmol) at rt and the mixture stirred at rt for 48 h. After completion of reaction (by TLC), water (10 mL) was added and a white precipitate formed. The reaction mixture was filtered and solid was washed with water to obtain the desired product as white solid (1.40 g, 41%). MS: 354.18 [M+H]+

Aufarbeitung

  1. additionwas added
  2. customa white precipitate formed
  3. filtrationThe reaction mixture was filtered
  4. washsolid was washed with water

Quellen und Nachweise

ORD-Eintrag
ord-2a107e64ce68453ea23c0c90efdfd565
Quelldatensatz
uspto-grants-2015_11
Patentnummer
US09181234B2

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