Ammonium Hydroxide → 4-Chloro-3-iodo-5-nitropyridin-2-amine

HRID 1969554노트

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HRID 1969554 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9].[N+:10]([O-])([O-:12])=[O:11].[K+].[OH-].[NH4+]>OS(O)(=O)=O>[Cl:1][C:2]1[C:7]([N+:10]([O-:12])=[O:11])=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9]

참가 물질

5

반응물 3

HCID 14923Ammonium Hydroxide2회HCID 24434Potassium NitrateHCID 229365964-Chloro-3-iodopyridin-2-amine

생성물 1

HCID 585571744-Chloro-3-iodo-5-nitropyridin-2-amine수율 29%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

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온도
0 °C

실험 절차

A solution of 4-chloro-3-iodopyridin-2-amine (0.25 g, 0.982 mmol, Boa Pharma) in concd H2SO4 (1.95 mL) was cooled to about 0° C. before the portion wise addition of potassium nitrate (0.21 g, 2.2 mmol) over 10 min. The reaction was stirred for about 4 h at about 0° C. The reaction mixture was slowly pipetted over a solution of ammonium hydroxide and crushed ice (10 mL) in an ice bath. The pH of the reaction was maintained above 9 by the incremental addition of ammonium hydroxide. The resulting precipitate was filtered and dried to afford 4-chloro-3-iodo-5-nitropyridin-2-amine (0.085 g, 29%) as a green-tinted solid LC/MS (Table 1, Method n) Rt=0.64 min; MS m/z: 298 (M−H)−.

후처리

  1. filtrationThe resulting precipitate was filtered
  2. customdried

출처 및 근거

ORD 기록
ord-b2ef1b06269a4d58ba3777385eacc390
출처 데이터셋
uspto-grants-2013_04
특허 번호
US08426411B2

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