Sulfur → HCID 12891716, Verbindung

HRID 1856566Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1856566
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][C:9]([N:11]([CH2:26][CH3:27])[CH:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:14][CH2:13]1)=S.[S]>[Hg]=O.CO>[CH2:26]([N:11]([CH:12]1[CH2:17][CH2:16][N:15]([CH2:18][CH2:19][C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH2:14][CH2:13]1)[C:9]1[NH:8][C:3]2[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=2[N:1]=1)[CH3:27]

Komponenten

5

Edukt 2

HCID 5362487SulfurHCID 12891715HCID 12891715, Verbindung

Produkt 1

HCID 12891716HCID 12891716, VerbindungAusbeute 43 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 30856Mercuric oxideKatalysatorHCID 887MethanolLösungsmittel

Versuchsvorschrift

A mixture of 39.8 parts of N-(2-aminophenyl)-N'-ethyl-N'-[I-(2-phenylethyl)-4-piperidinyl]thiourea, 15 parts of mercury oxide, 0.1 parts of sulfur and 400 parts of methanol is stirred and refluxed overnight. The reaction mixture is filtered hot over Hyflo and the filtrate is evaporated. The residue is crystallized from 4-methyl-2-pentanone. The product is filtered off and dried, yielding 14.5 parts (43%) of N-ethyl-N-[I-(2-phenylethyl)-4-piperidinyl]-1H-benzimidazol-2-amine; mp. 204.9° C.

Aufarbeitung

  1. temperaturerefluxed overnight
  2. filtrationThe reaction mixture is filtered hot over Hyflo
  3. customthe filtrate is evaporated
  4. customThe residue is crystallized from 4-methyl-2-pentanone
  5. filtrationThe product is filtered off
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-1c6ea741abcc417cafc6a1c603e576f2
Quelldatensatz
uspto-grants-1980_08
Patentnummer
US04219559

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