2-Bromo-1-(thiophen-2-yl)ethan-1-one → HCID 178488931, Verbindung

HRID 235952

Reaktionsgleichung

Reaktionsgleichung von HRID 235952
[CH3:1][O:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([NH2:9])=[NH:8])=[CH:5][C:4]=1[CH3:12].Br[CH2:14][C:15]([C:17]1[S:18][CH:19]=[CH:20][CH:21]=1)=O>C(Cl)(Cl)Cl>[CH3:12][C:4]1[CH:5]=[C:6]([C:7]2[NH:9][CH:14]=[C:15]([C:17]3[S:18][CH:19]=[CH:20][CH:21]=3)[N:8]=2)[CH:10]=[CH:11][C:3]=1[O:2][CH3:1]

Komponenten

4

Edukt 2

HCID 27763722-Bromo-1-(thiophen-2-yl)ethan-1-oneHCID 13621616HCID 13621616, Verbindung

Produkt 1

HCID 178488931HCID 178488931, VerbindungAusbeute 79,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel2×

Versuchsvorschrift

A slurry of 22 (21.6 g, 0.132 mol) in CHCl3 (300 ml) was treated dropwise over 15 minutes with 2-(bromoacetyl)-thiophene (10.84, 0.0476 mol, 92% pure) in CHCl3 (55 ml). The reaction mixture was stirred at room temperature for 24 hours, and then filtered to remove 10.2 g of the hydrobromide of 22. The mother liquors were concentrated to a semisolid which was swirled with 75 ml of methylene chloride and refrigerated overnight. The resultant gray solid was washed with CH2Cl2 and dried to give 10.2 grams (79%) of 23; m.p. 110°-114°. The analytical sample was dried in vacuo at 85°, m.p. 115°-117°.

Aufarbeitung

  1. filtrationfiltered
  2. customto remove 10.2 g of the hydrobromide of 22
  3. concentrationThe mother liquors were concentrated to a semisolid which
  4. customwas swirled with 75 ml of methylene chloride and refrigerated overnight
  5. washThe resultant gray solid was washed with CH2Cl2
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-aec3976a66fd4ea9bb7db81c5a2eb469
Quelldatensatz
uspto-grants-1987_02
Patentnummer
US04642311

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