Methane → 5-Bromoimidazo-[1,2-a]-quinoline-2-carboxylic acid

HRID 1277970ノート

反応式

HRID 1277970 の反応式
[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]2[CH:12]=[C:13]([C:15]([O:17]CC)=[O:16])[N:14]=[C:4]2[CH:3]=1.[OH-].[Na+].Cl.C>O.C(O)C.C(Cl)(Cl)Cl.CO>[Br:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]2[CH:12]=[C:13]([C:15]([OH:17])=[O:16])[N:14]=[C:4]2[CH:3]=1

参加物

9

反応物 4

HCID 297MethaneHCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 12763980Ethyl 5-bromoimidazo-[1,2-a]-quinoline-2-carboxylate

生成物 1

HCID 127639795-Bromoimidazo-[1,2-a]-quinoline-2-carboxylic acid

試薬・触媒・溶媒 4

HCID 702Ethanol溶媒HCID 887Methanol溶媒HCID 962Water溶媒HCID 6212Chloroform溶媒

実験手順

1.28 g of ethyl 5-bromoimidazo-[1,2-a]-quinoline-2-carboxylate were heated on a steam bath with 5 ml of 1 N sodium hydroxide solution in 20 ml of water and 50 ml of ethanol until a clear solution was obtained (approx. 15 mins). 5 ml of 1 N hydrochloric acid were then added thereto and the solution was allowed to cool slowly to room temperature. The pale green crystals thus formed were filtered off and were washed with methanol. The mother liquors were reduced in volume and cooled to give a second crop. The two crops were combined in 50 ml of chloroform and 50 methanol and the solution obtained was decolorized with charcoal. The solution was reduced in volume under vacuum and the residue was cooled in ice to give colorless plates of 5-bromoimidazo-[1,2-a]-quinoline-2-carboxylic acid melting at 288°-90° C. (decomp).

後処理

  1. customwas obtained (approx. 15 mins)
  2. customThe pale green crystals thus formed
  3. filtrationwere filtered off
  4. washwere washed with methanol
  5. temperaturecooled
  6. customto give a second crop
  7. temperaturethe residue was cooled in ice

出典と根拠

ORDレコード
ord-1264cf640d914490ad1cae440b157eb7
出典データセット
uspto-grants-1981_07
特許番号
US04279912

反応ノート

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