Methane → N,N'-Dibutylcarbamimidothioic acid(3-methyl-2-quinoxalinyl)ester, hydrochloride

HRID 1702837

Reaktionsgleichung

Reaktionsgleichung von HRID 1702837
[Cl:1][C:2]1[C:11]([CH3:12])=[N:10][C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.C.[CH2:14]([NH:18][C:19]([NH:21][CH2:22][CH2:23][CH2:24][CH3:25])=[S:20])[CH2:15][CH2:16][CH3:17]>CO>[ClH:1].[CH3:12][C:11]1[C:2]([S:20][C:19](=[N:18][CH2:14][CH2:15][CH2:16][CH3:17])[NH:21][CH2:22][CH2:23][CH2:24][CH3:25])=[N:3][C:4]2[C:9]([N:10]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2

Komponenten

5

Edukt 3

HCID 297MethaneHCID 2362762-Chloro-3-methylquinoxalineHCID 2723622N,N'-Dibutylthiourea

Produkt 1

HCID 131712828N,N'-Dibutylcarbamimidothioic acid(3-methyl-2-quinoxalinyl)ester, hydrochloride

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel2×

Versuchsvorschrift

2-Chloro-3-methylquinoxaline (3.572 g., 0.02 mole) was dissolved in 50 ml. of methanol, treated with Norit and filtered. The filtrate was added to 3.767 g. (0.02 mole) of 1,3-dibutylthiourea dissolved in 25 ml. of methanol. The resulting solution was stirred at room temperature for 1 hour and evaporated on a rotary evaporator. The residual oil was triturated successively with several portions of ether, 2:1 pentane-ether and acetone, and was filtered and washed with pentane, to give 2.60 g. (38.6%) of product as a tan solid, m.p. 97°-99°.

Aufarbeitung

  1. filtrationfiltered
  2. additionThe filtrate was added to 3.767 g
  3. customevaporated on a rotary evaporator
  4. customThe residual oil was triturated successively with several portions of ether, 2:1 pentane-ether and acetone
  5. filtrationwas filtered
  6. washwashed with pentane
  7. customto give 2.60 g

Quellen und Nachweise

ORD-Eintrag
ord-f8cb6406fcb04e8689a3ebcf483ab84b
Quelldatensatz
uspto-grants-1982_09
Patentnummer
US04349674

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