2-Amino-5-bromopyridine → HCID 23158249、化合物

HRID 601692ノート

反応式

HRID 601692 の反応式
Cl[CH2:2][CH2:3][C:4](=O)[CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7].[NH2:12][C:13]1[CH:18]=[CH:17][C:16]([Br:19])=[CH:15][N:14]=1>C(O)C>[Br:19][C:16]1[CH:17]=[CH:18][C:13]2[N:14]([CH:2]=[C:3]([CH2:4][CH2:5][C:6]([O:8][CH2:9][CH3:10])=[O:7])[N:12]=2)[CH:15]=1

参加物

4

反応物 2

HCID 706222-Amino-5-bromopyridineHCID 23158165Ethyl 5-chloro-3-oxopentanoate

生成物 1

HCID 23158249HCID 23158249、化合物収率 13,903.8%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4.28 mg of ethyl 5-chloro-3-oxopentanoate was dissolved in 40 ml of ethanol, 2.94 g of 2-amino-5-bromopyridine was added and the mixture was stirred all night by heating under reflux. The mixture was cooled down to room temperature, and the solvents were distilled outunder reduced pressure. Ethyl acetate followed by saturated sodium bicarbonate aqueous solution were added. Organic layer was dried with anhydrous sodium sulfate, and the solvents were distilled outunder reduced pressure. The obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=50:50) to obtain 990 mg of the above compound as crude product.

後処理

  1. temperatureby heating
  2. temperatureunder reflux
  3. distillationthe solvents were distilled outunder reduced pressure
  4. additionwere added
  5. dry with materialOrganic layer was dried with anhydrous sodium sulfate
  6. distillationthe solvents were distilled outunder reduced pressure
  7. customThe obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=50:50)

出典と根拠

ORDレコード
ord-3a4e54da656f4d77a75691cfecfd2013
出典データセット
uspto-grants-2011_03
特許番号
US07902369B2

反応ノート

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