2-Cyanoethanethioamide → HCID 178510482, Verbindung

HRID 2362819Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2362819
[N:1]([CH2:4][CH2:5][O:6][C:7]1[CH:18]=[CH:17][C:10]([CH:11]=[C:12]([C:15]#[N:16])[C:13]#[N:14])=[CH:9][CH:8]=1)=[N+:2]=[N-:3].[C:19]([CH2:21][C:22]([NH2:24])=[S:23])#[N:20]>C(O)C>[NH2:16][C:15]1[C:12]([C:13]#[N:14])=[C:11]([C:10]2[CH:17]=[CH:18][C:7]([O:6][CH2:5][CH2:4][N:1]=[N+:2]=[N-:3])=[CH:8][CH:9]=2)[C:21]([C:19]#[N:20])=[C:22]([SH:23])[N:24]=1

Komponenten

4

Versuchsvorschrift

A solution of 2.39 g (9.98 mmol) of the compound from Example 37A and 2.50 g (24.92 mmol) of cyanothioacetamide in 100 ml of ethanol is stirred at +78° C. for 6 h. After cooling to RT and a further 12 h of standing without stirring, the reaction mixture is concentrated using a rotary evaporator. The residue is recrystallized from about 30 ml of ethanol. The resulting precipitate is filtered off with suction and washed twice with in each case 10 ml of methyl tert-butyl ether.

Aufarbeitung

  1. concentrationthe reaction mixture is concentrated
  2. customa rotary evaporator
  3. customThe residue is recrystallized from about 30 ml of ethanol
  4. filtrationThe resulting precipitate is filtered off with suction
  5. washwashed twice with in each case 10 ml of methyl tert-butyl ether

Quellen und Nachweise

ORD-Eintrag
ord-b01065bebd994833b94fcaac08b370c1
Quelldatensatz
uspto-grants-2014_04
Patentnummer
US08691850B2

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