Glycolic Acid → 2-Hydroxymethyl-3-methyl-5-phenylimidazo[5,4-b]pyridine

HRID 1599343ノート

反応式

HRID 1599343 の反応式
[NH2:1][C:2]1[C:3]([NH:14][CH3:15])=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][CH:7]=1.[C:16]([OH:20])(=O)[CH2:17]O>>[OH:20][CH2:16][C:17]1[N:14]([CH3:15])[C:3]2[C:2]([N:1]=1)=[CH:7][CH:6]=[C:5]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[N:4]=2

参加物

3

反応物 2

HCID 757Glycolic AcidHCID 108456893-Amino-2-methylamino-6-phenylpyridine

生成物 1

HCID 108475892-Hydroxymethyl-3-methyl-5-phenylimidazo[5,4-b]pyridine収率 15.3%

実験手順

A procedure similar to that described in Preparation 43 was repeated, except that 4.9 g of 3-amino-2-methylamino-6-phenylpyridine (prepared as described in Preparation 109) and 5.6 g of glycolic acid were used, and that the product was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of ethyl acetate and ethanol in ratios ranging from 1:0 to 10:1 by volume as the eluent, to give 0.9 g of the title compound, melting at 174°-177° C.

後処理

  1. customA procedure similar to that described in Preparation 43
  2. customthat the product was purified by column chromatography through silica gel
  3. washa gradient elution method

出典と根拠

ORDレコード
ord-81c328c43347453092ab9d40dbffdde7
出典データセット
uspto-grants-1998_04
特許番号
US05739345

反応ノート

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