Ammonia → 4-Chloropyridine-2,3-diamine

HRID 1728576노트

반응식

HRID 1728576 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

HCID 224180044-Chloropyridine-2,3-diamine

시약·촉매·용매 2

HCID 23925Iron촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7d1fb2ca567d40f681e8fddddd11008f
출처 데이터셋
uspto-grants-1994_07
특허 번호
US05328911

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