Dichloromethane → HCID 13457850, Verbindung

HRID 463542Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 463542
C(Cl)Cl.[SH:4][C:5]1[N:9]([CH3:10])[C:8]2[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=2[N:6]=1.Br[CH:16]([C:20]1[CH:25]=[CH:24][C:23]([Cl:26])=[CH:22][CH:21]=1)[C:17]([OH:19])=[O:18]>C(N(CC)CC)C>[Cl:26][C:23]1[CH:22]=[CH:21][C:20]([CH:16]([S:4][C:5]2[N:9]([CH3:10])[C:8]3[CH:11]=[CH:12][CH:13]=[CH:14][C:7]=3[N:6]=2)[C:17]([OH:19])=[O:18])=[CH:25][CH:24]=1

Komponenten

5

Edukt 3

HCID 6344DichloromethaneHCID 10490868alpha-Bromo-4-chlorophenylacetic acidHCID 178481665HCID 178481665, Verbindung

Produkt 1

HCID 13457850HCID 13457850, VerbindungAusbeute 41 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

A methylene chloride solution of 3.3 g (0.02M) of 2-mercapto-1-methyl-1H-benzimidazole, 5.0 g (0.02M) of α-bromo-(p-chlorophenyl)acetic acid and 4.0 g (0.04M) of triethylamine is heated to reflux overnight. The reaction mixture is neutralized with a diluted HCL solution. The layers are separated and the organic layer is dried over anhydrous magnesium sulfate. After removal of methylene chloride the residue is recrystallized from acetonitrile. The recrystallized material weighs 4.1 g (41% yield) and has a melting point of 161°-3° C. dec.

Aufarbeitung

  1. temperatureto reflux overnight
  2. customThe layers are separated
  3. dry with materialthe organic layer is dried over anhydrous magnesium sulfate
  4. customAfter removal of methylene chloride the residue
  5. customis recrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-d0ca4776a20d40edbe0eb7f5c3e47d45
Quelldatensatz
uspto-grants-1985_05
Patentnummer
US04520196

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