Dichloromethane → HCID 19989845, Verbindung

HRID 973419

Reaktionsgleichung

Reaktionsgleichung von HRID 973419
[CH3:1][N:2]1[CH2:6][CH2:5][CH:4]([C:7]2[NH:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]=2)[CH2:3]1.C(Cl)(Cl)=[O:17].C1(C)C=CC=CC=1.C(N(CC)CC)C.[CH2:34]([Cl:36])Cl>>[Cl:36][CH2:34][CH2:5][CH:4]1[C:7]2=[N:11][C:10]3[CH:12]=[CH:13][CH:14]=[CH:15][C:9]=3[N:8]2[C:1](=[O:17])[N:2]([CH3:6])[CH2:3]1

Komponenten

5

Edukt 4

HCID 6344Dichloromethane2×HCID 8471TriethylamineHCID 19083224Phosgen tolueneHCID 19989862HCID 19989862, Verbindung

Produkt 1

HCID 19989845HCID 19989845, Verbindung

Versuchsvorschrift

A solution of 4 g (0.02 mol) of 2-(1-methyl-3-pyrrolidinyl)-1H-benzimidazole in 100 mL of CH2Cl2 was added dropwise to a solution of 12.5 (0.025 mol) of 20% phosgene/toluene in 30 mL of CH2Cl2. The solution was stirred for 2 h, and 10 g (0.1 mol) of triethylamine was added dropwise. Stirring was continued for 2 h and the solution was extracted with dilute NaOH. The organic layer was dried (Na2SO4) and concentrated. The residue was crystallized twice from isopropyl ether. Yield 1.5 g (28%), mp 88°-91° C.

Aufarbeitung

  1. stirringStirring
  2. waitwas continued for 2 h
  3. extractionthe solution was extracted with dilute NaOH
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. concentrationconcentrated
  6. customThe residue was crystallized twice from isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-27f19568d9bd4b42a0e6cf1e47ac43b7
Quelldatensatz
uspto-grants-1991_11
Patentnummer
US05063228

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