2,6-Dimethoxypyridine-3-carboxylic acid → HCID 10483696, Verbindung

HRID 720658

Reaktionsgleichung

Reaktionsgleichung von HRID 720658
[CH3:1][O:2][C:3]1[N:11]=[C:10]([O:12][CH3:13])[CH:9]=[CH:8][C:4]=1[C:5]([OH:7])=O.[CH:14]1([CH2:17][N:18]2[C:26]3[N:25]=[C:24]([CH2:27][C:28]4[CH:33]=[CH:32][C:31]([NH:34][CH3:35])=[CH:30][CH:29]=4)[NH:23][C:22]=3[C:21](=[O:36])[N:20]([CH2:37][C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=3[F:44])[C:19]2=[O:45])[CH2:16][CH2:15]1>CN(C)C1C=CN=CC=1.C(N(CC)CC)C>[CH:14]1([CH2:17][N:18]2[C:26]3[N:25]=[C:24]([CH2:27][C:28]4[CH:29]=[CH:30][C:31]([N:34]([CH3:35])[C:5](=[O:7])[C:4]5[CH:8]=[CH:9][C:10]([O:12][CH3:13])=[N:11][C:3]=5[O:2][CH3:1])=[CH:32][CH:33]=4)[NH:23][C:22]=3[C:21](=[O:36])[N:20]([CH2:37][C:38]3[CH:43]=[CH:42][CH:41]=[CH:40][C:39]=3[F:44])[C:19]2=[O:45])[CH2:16][CH2:15]1

Komponenten

5

Edukt 2

HCID 8531782,6-Dimethoxypyridine-3-carboxylic acidHCID 218916913-Cyclopropylmethyl-8-[4-(methylamino)-benzyl]-1-(2-fluorobenzyl)-3,7-dihydropurine-2,6-dione

Produkt 1

HCID 10483696HCID 10483696, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 142844-(Dimethylamino)pyridineKatalysatorHCID 8471TriethylamineLösungsmittel

Versuchsvorschrift

This compound was prepared by a method similar to that described in example 79 except that 2,6-dimethoxynicotinic acid (Aldrich) was used in place of N-acetyl-6-amino-2-pyridine carboxylic acid, the reaction was performed using 1 equivalent of 3-cyclopropylmethyl-8-[4-(methylamino)-benzyl]-1-(2-fluorobenzyl)-3,7-dihydropurine-2,6-dione and excess triethylamine and a catalytic amount of 4-dimethylaminopyridine were added as the final reagents to the reaction mixture. The product was purified by chromatography using silica gel eluted with 9:1 ethyl acetate/hexanes followed by crystallization from acetonitrile. MS, m/z(M+)=599.2417.

Aufarbeitung

  1. customThis compound was prepared by a method similar to
  2. customThe product was purified by chromatography
  3. washeluted with 9:1 ethyl acetate/hexanes
  4. customfollowed by crystallization from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-e5afa1cbea114ad0b7e8d26af3b39261
Quelldatensatz
uspto-grants-2006_11
Patentnummer
US07135475B2

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