Ammonia → HCID 178420422、化合物

HRID 333749

反応式

HRID 333749 の反応式
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12](O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:15][C:16]1[C:21]([NH2:22])=[CH:20][CH:19]=[CH:18][N:17]=1.N>>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]1[NH:15][C:16]2=[N:17][CH:18]=[CH:19][CH:20]=[C:21]2[N:22]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

参加物

4

反応物 3

HCID 222AmmoniaHCID 99562,3-DiaminopyridineHCID 5622014-(Benzyloxy)butanoic acid

生成物 1

HCID 178420422HCID 178420422、化合物収率 86%

実験手順

4-(Benzyloxy)butanoic acid (5.0 g) and 2,3-diaminopyridine (1.12 g) were stirred at 150° C. for 10 hr. Under ice-cooling, to the reaction mixture was added concentrated aqueous ammonia, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.36 g).

後処理

  1. temperatureUnder ice-cooling, to the reaction mixture
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-257fd407c9e749c5858e8bd50352b094
出典データセット
uspto-grants-2014_11
特許番号
US08883788B2

関連ノート

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