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Methane → HCID 10376941, Verbindung

HRID 1701880
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1701880
[CH3:1][NH2:2].[N:3]1[CH:8]=[CH:7][CH:6]=[C:5]([C:9]2([C:14]([S:16]C)=S)[CH2:13][CH2:12][CH2:11][S:10]2)[CH:4]=1.C>C(O)C>[CH3:1][NH:2][C:14]([C:9]1([C:5]2[CH:4]=[N:3][CH:8]=[CH:7][CH:6]=2)[CH2:13][CH2:12][CH2:11][S:10]1)=[S:16]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 297MethaneHCID 6329MethylamineHCID 13043956Methyl 2-(pyridin-3-yl)thiolane-2-carbodithioate

Produkt 1

HCID 10376941HCID 10376941, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel3×

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

A 33% (weight/volume) solution of methylamine in ethanol (11 cc) is added dropwise, in the course of 5 minutes, to a solution of methyl 2-(pyrid-3-yl)-tetrahydrothiophen-2-carbodithioate (14.3 g) in ethanol (50 cc), kept at a temperature of about 20° C. The solution is subsequently stirred for 5 hours at the same temperature and then cooled to 0° C. The resulting crystals are filtered off, washed with ethanol (8 cc) and then twice with diisopropyl ether (20 cc in total) and dried under reduced pressure (20 mm Hg; 2.7 kPa) at 20° C. The product thus obtained (7.2 g) is dissolved in boiling ethanol (35 cc); decolourising charcoal (0.4 g) is added to the solution, which is filtered hot, and the filtrate is then cooled for 1 hour at a temperature of about 5° C. The resulting crystals are filtered off, washed with ethanol (5 cc) and then twice with diisopropyl ether (14 cc in total) and dried under reduced pressure (1 mm Hg; 0.13 kPa) at 40° C. N-Methyl-2-(pyrid-3-yl)-tetrahydrothiophen-2-carbothioamide (5.8 g), melting at 133° C., is thus obtained.

Aufarbeitung

  1. customkept at a temperature of about 20° C
  2. filtrationThe resulting crystals are filtered off
  3. washwashed with ethanol (8 cc)
  4. dry with materialtwice with diisopropyl ether (20 cc in total) and dried under reduced pressure (20 mm Hg; 2.7 kPa) at 20° C
  5. customThe product thus obtained (7.2 g)
  6. dissolutionis dissolved
  7. filtrationis filtered hot
  8. temperaturethe filtrate is then cooled for 1 hour at a temperature of about 5° C
  9. filtrationThe resulting crystals are filtered off
  10. washwashed with ethanol (5 cc)
  11. dry with materialtwice with diisopropyl ether (14 cc in total) and dried under reduced pressure (1 mm Hg; 0.13 kPa) at 40° C

Quellen und Nachweise

ORD-Eintrag
ord-eba34a5eb9e94ff5a8fef4ac7761532d
Quelldatensatz
uspto-grants-1983_04
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04379154

Notizen zur Reaktion

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