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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 371931
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HRID 371931 반응식
[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
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참가 물질

7

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 241
Benzene
용매
HCID 8058Hexane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-6eb54cdca7844479a6ed7f56aef8c9ff
출처 데이터셋
uspto-grants-1978_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04088654

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