5-Chlorovaleronitrile → S-(4-cyanobutyl)isothiourea hydrochloride

HRID 2196461Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2196461
[Cl:1][CH2:2][CH2:3][CH2:4][CH2:5][C:6]#[N:7].[NH2:8][C:9]([NH2:11])=[S:10]>O>[ClH:1].[C:6]([CH2:5][CH2:4][CH2:3][CH2:2][S:10][C:9](=[NH:8])[NH2:11])#[N:7]

Komponenten

4

Versuchsvorschrift

The 5-chloropentanenitrile (5.68 g, 48.3 mmol) and thiourea (4.04 g, 53.1 mmol) are mixed in 40 ml of water. The mixture is heated to reflux for 3 to 4 hours. The reaction mixture is evaporated and 20 ml of ethanol are added and then evaporated as well. This is repeated three times. After that, 10 ml of methanol and 30 ml of acetone are added and the mixture is stirred for one hour. The crystalline material is filtered and the product is dried under high vacuum overnight to yield S-(4-cyanobutyl)isothiourea hydrochloride.

Aufarbeitung

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 3 to 4 hours
  3. customThe reaction mixture is evaporated
  4. addition20 ml of ethanol are added
  5. customevaporated as well
  6. additionAfter that, 10 ml of methanol and 30 ml of acetone are added
  7. filtrationThe crystalline material is filtered
  8. customthe product is dried under high vacuum overnight

Quellen und Nachweise

ORD-Eintrag
ord-5cb3a0da2b544d7b9ff2ec2c9d6dc9b4
Quelldatensatz
uspto-grants-2012_12
Patentnummer
US08338454B2

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