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Pyridine → HCID 18923456、化合物

HRID 1290179
ノート
印刷プレビュー

反応式

HRID 1290179 の反応式
Cl.Cl.[NH2:3][C:4]1[C:5]([Cl:24])=[C:6]([C:20]([Cl:23])=[CH:21][CH:22]=1)[CH2:7][O:8][C:9]1[C:10]2[N:11]([C:15]([Br:19])=[C:16]([CH3:18])[N:17]=2)[CH:12]=[CH:13][CH:14]=1.N1C=CC=CC=1.[CH2:31]([N:33]=[C:34]=[O:35])[CH3:32]>CN1CCCC1=O>[Br:19][C:15]1[N:11]2[CH:12]=[CH:13][CH:14]=[C:9]([O:8][CH2:7][C:6]3[C:20]([Cl:23])=[CH:21][CH:22]=[C:4]([NH:3][C:34]([NH:33][CH2:31][CH3:32])=[O:35])[C:5]=3[Cl:24])[C:10]2=[N:17][C:16]=1[CH3:18]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 8022Ethyl isocyanateHCID 189233178-(3-Amino-2,6-dichlorobenzyloxy)-3-bromo-2-methylimidazo[1,2-a]pyridine dihydrochloride

生成物 1

HCID 18923456HCID 18923456、化合物

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
60 °C

実験手順

To a mixture of 8-(3-amino-2,6-dichlorobenzyloxy)-3-bromo-2-methylimidazo[1,2-a]pyridine dihydrochloride (100 mg), pyridine (0.5 ml) and N-methylpyrrolidone (1.5 ml) was added ethyl isocyanate (0.10 ml). The mixture was stirred at 60° C. for 6 hours. The insoluble material was filtered off and washed with water. The filtrate and washings were combined and separated precipitate was collected by filtration. The precipitate was purified by preparative thin-layer chromatography (20% solution of methanol in dichloromethane) followed by recrystallization from n-hexane to give 3-bromo-8-[2,6-dichloro-3-(N'-ethylureido)benzyloxy]-2-methylimidazo[1,2-a]pyridine (13 mg) as crystals.

後処理

  1. filtrationThe insoluble material was filtered off
  2. washwashed with water
  3. customseparated precipitate
  4. filtrationwas collected by filtration
  5. customThe precipitate was purified by preparative thin-layer chromatography (20% solution of methanol in dichloromethane)
  6. customfollowed by recrystallization from n-hexane

出典と根拠

ORDレコード
ord-01b2ef26d8bb4782877fb4568484cd31
出典データセット
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05750699

反応ノート

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