Ethyl bromoacetate → 6-chloro-2-ethyl-1-ethoxycarbonylmethyl-1H-imidazo[4,5-b]quinoxaline

HRID 2397548

反応式

HRID 2397548 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]1[NH:12][C:13]([CH2:15][CH3:16])=[N:14][C:6]1=[N:5]2.C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26]>CN(C)C=O>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]1[N:12]([CH2:24][C:25]([O:27][CH2:28][CH3:29])=[O:26])[C:13]([CH2:15][CH3:16])=[N:14][C:6]1=[N:5]2

参加物

5

反応物 3

HCID 7748Ethyl bromoacetateHCID 11430Potassium CarbonateHCID 1784375416-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline

生成物 1

HCID 214359666-chloro-2-ethyl-1-ethoxycarbonylmethyl-1H-imidazo[4,5-b]quinoxaline

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 100 parts of 6-chloro-2-ethyl-1H-imidazo[4,5-b]quinoxaline, 70 parts of anhydrous potassium carbonate, 75 parts of ethyl bromoacetate, and 600 parts of anhydrous dimethylformamide was heated at 100° for 2.5 hours. The mixture was filtered and the crude product was precipitated from the filtrate by addition of 1200 parts of water, collected by filtration, washed with water, ethanol, and ether, and airdried. Recrystallization from 95% ethanol afforded 63 parts of 6-chloro-2-ethyl-1-ethoxycarbonylmethyl-1H-imidazo[4,5-b]quinoxaline, m.p. 174°-175°.

後処理

  1. temperaturewas heated at 100° for 2.5 hours
  2. filtrationThe mixture was filtered
  3. customthe crude product was precipitated from the filtrate by addition of 1200 parts of water
  4. filtrationcollected by filtration
  5. washwashed with water, ethanol, and ether
  6. customRecrystallization from 95% ethanol

出典と根拠

ORDレコード
ord-2d02fb0618364871867ce677d5505903
出典データセット
uspto-grants-1977_05
特許番号
US04022777

関連ノート

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