1,2-Dimethoxyethane → Pyridine-2,3-dicarboxamide

HRID 330361Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 330361
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.ClC[C:11]([NH:13]C(C)(C)CC(C)(C)C)=[O:12].C(N(C(C)C)CC)(C)C.C(COC)[O:32]C>C(Cl)Cl>[N:4]1[CH:5]=[CH:6][CH:7]=[C:8]([C:11]([NH2:13])=[O:12])[C:3]=1[C:2]([NH2:1])=[O:32]

Komponenten

6

Edukt 4

HCID 80711,2-DimethoxyethaneHCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 3524332-chloro-N-(1,1,3,3-tetramethylbutyl)acetamide

Produkt 1

HCID 578921Pyridine-2,3-dicarboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Pyridine diamide 4 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.011 mol), 2-chloro-N-(1,1,3,3,-tetramethylbutyl)acetamide (0.033 mol), diisopropylethylamine (0.025 mol) and dimethoxyethane (25 mL). The product was isolated from the methylene chloride extraction of the acidic aqueous layer. The product was made basic by extraction of the methylene chloride solution with aqueous NaOH. The methylene chloride solution was concentrated, and the residue was distilled (150° C., 0.03 mm) to afford 3.7 g of pure product.

Aufarbeitung

  1. extractionThe product was made basic by extraction of the methylene chloride solution with aqueous NaOH
  2. concentrationThe methylene chloride solution was concentrated
  3. distillationthe residue was distilled (150° C., 0.03 mm)

Quellen und Nachweise

ORD-Eintrag
ord-31842623b17d4ff58481920f0a65a183
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04895951

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