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

HRID 330364Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 330364
[NH2:1][CH2:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1.ClC[C:11]([N:13](C(C)C)C(C)C)=[O:12].C(N(C(C)C)CC)(C)C.C(COC)[O:30]C>>[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:30]

Komponenten

5

Edukt 4

HCID 80711,2-DimethoxyethaneHCID 195092-PyridinemethanamineHCID 81531DiisopropylethylamineHCID 1390132-chloro-N,N-bis(propan-2-yl)acetamide

Produkt 1

HCID 578921Pyridine-2,3-dicarboxamide

Versuchsvorschrift

Pyridine diamide 7 was prepared according to the general procedure described in Example 8 using 2-(aminomethyl)pyridine (0.013 mol), 2-chloro-N,N-diisopropylacetamide (0.038 mol), diisopropylethylamine (0.038 mol) and dimethoxyethane (25 mL). The product was isolated from both the methylene chloride extraction of the acidic aqueous layer and the heptane extraction of the basic layer in about equal amounts. Mass spectral analysis of the two layers showed the material in the heptane layer to be of greater purity. The residue from the heptane layer was distilled (150° C., 0.05 mm) to afford 2.2 g of product.

Aufarbeitung

  1. customThe product was isolated from both
  2. extractionthe methylene chloride extraction of the acidic aqueous layer
  3. extractionthe heptane extraction of the basic layer in about equal amounts
  4. distillationThe residue from the heptane layer was distilled (150° C., 0.05 mm)

Quellen und Nachweise

ORD-Eintrag
ord-664d61f0a549455c90c7133988cca0cf
Quelldatensatz
uspto-grants-1990_01
Patentnummer
US04895951

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