Ammonia → 4-Chloropyridine-2,3-diamine

HRID 1728576ノート

反応式

HRID 1728576 の反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([Cl:11])[CH:5]=[CH:4][N:3]=1.Cl.N>[Fe].CO>[Cl:11][C:6]1[CH:5]=[CH:4][N:3]=[C:2]([NH2:1])[C:7]=1[NH2:8]

参加物

6

反応物 3

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 40716944-Chloro-3-nitropyridin-2-amine

生成物 1

HCID 224180044-Chloropyridine-2,3-diamine

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 887Methanol溶媒

実験手順

3.6 g of 2-amino-4-chloro-3-nitropyridine was added to 21 ml of methanol and 24 ml of concentrated hydrochloric acid, and the mixture was vigorously stirred. Powdery iron was added in small portions to the mixture. 10 min after the completion of the addition, the mixture was poured into an iced concentrated aqueous ammonia and extracted with ethyl acetate. The extract was dried over magnesium sulfate, and the solvent was distilled off in vacuo. The residue was purified by silica gel chromatography (CH2Cl2 :MeOH=20:1-10:1) to prepare 2.6 g of 4-chloro-2,3-diaminopyridine as a purplish white crystal.

後処理

  1. addition10 min after the completion of the addition
  2. extractionextracted with ethyl acetate
  3. dry with materialThe extract was dried over magnesium sulfate
  4. distillationthe solvent was distilled off in vacuo
  5. customThe residue was purified by silica gel chromatography (CH2Cl2 :MeOH=20:1-10:1)
  6. customto prepare 2.6 g of 4-chloro-2,3-diaminopyridine as a purplish white crystal

出典と根拠

ORDレコード
ord-7d1fb2ca567d40f681e8fddddd11008f
出典データセット
uspto-grants-1994_07
特許番号
US05328911

反応ノート

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