2-Amino-5-bromopyridine → HCID 23158249, 화합물

HRID 601692노트

반응식

HRID 601692 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 23158249HCID 23158249, 화합물수율 13,903.8%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-3a4e54da656f4d77a75691cfecfd2013
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07902369B2

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