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Sodium Carbonate → 7-[3-(Dimethylamino)propoxy]-3,5-dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid, ethyl ester

HRID 1415147
ノート
印刷プレビュー

反応式

HRID 1415147 の反応式
[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][OH:6].C([Li])CCC.Cl[C:14]1[C:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:18]([CH3:25])[N:17]=[C:16]2[N:26]([CH3:29])[CH:27]=[N:28][C:15]=12.C(=O)([O-])[O-].[Na+].[Na+]>CCCCCC.C1C=CC=CC=1>[CH3:1][N:2]([CH3:7])[CH2:3][CH2:4][CH2:5][O:6][C:14]1[C:19]([C:20]([O:22][CH2:23][CH3:24])=[O:21])=[C:18]([CH3:25])[N:17]=[C:16]2[N:26]([CH3:29])[CH:27]=[N:28][C:15]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10340Sodium CarbonateHCID 766463-(Dimethylamino)-1-propanolHCID 123876407-chloro-3,5-dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid ethyl esterHCID 178418339Butyllithium

生成物 1

HCID 123876447-[3-(Dimethylamino)propoxy]-3,5-dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid, ethyl ester

試薬・触媒・溶媒 2

HCID 241
Benzene
溶媒
HCID 8058Hexane溶媒

実験手順

To a solution of 1.1 g. of 3-dimethylaminopropan-1-ol in 100 ml. of dry benzene are added 4 ml. of a 20% solution of butyl lithium in hexane. The mixture is stirred at room temperature for 15 minutes. After this time, 2.5 g. of 7-chloro-3,5-dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid, ethyl ester are added and the solution is heated at reflux temperature with stirring for 12 hours. After cooling, the solution is shaken with 50 ml. of a saturated aqueous sodium carbonate solution. The benzene layer is separated, dried with calcium chloride and evaporated to dryness. The remaining oily residue, 7-[3-(dimethylamino)propoxy]-3,5 -dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid, ethyl ester, is purified by distillation, yield 2.2 g. (85%); b.p. 175°-180° /0.01 mm.

後処理

  1. temperaturethe solution is heated
  2. temperatureat reflux temperature
  3. stirringwith stirring for 12 hours
  4. temperatureAfter cooling
  5. stirringthe solution is shaken with 50 ml
  6. customThe benzene layer is separated
  7. dry with materialdried with calcium chloride
  8. customevaporated to dryness
  9. distillationThe remaining oily residue, 7-[3-(dimethylamino)propoxy]-3,5 -dimethyl-3H-imidazo[4,5-b]pyridine-6-carboxylic acid, ethyl ester, is purified by distillation, yield 2.2 g

出典と根拠

ORDレコード
ord-2ba4b8ddd96d44cb86810fadaab0fbeb
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04003908

反応ノート

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