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Ammonium Chloride → 6-bromo-2-chloro-N3-methylpyridine-3,4-diamine

HRID 2209026
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HRID 2209026 반응식
[Br:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([NH:9][CH3:10])=[C:4]([N+:11]([O-])=O)[CH:3]=1.[Cl-].[NH4+]>C(O)C.O.CCOC(C)=O.[Fe]>[Br:1][C:2]1[N:7]=[C:6]([Cl:8])[C:5]([NH:9][CH3:10])=[C:4]([NH2:11])[CH:3]=1
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참가 물질

7

반응물 2

HCID 25517Ammonium ChlorideHCID 1178440196-bromo-2-chloro-N-methyl-4-nitropyridin-3-amine

생성물 1

HCID 1178428716-bromo-2-chloro-N3-methylpyridine-3,4-diamine

시약·촉매·용매 4

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매HCID 8857Ethyl Acetate용매

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온도
140 °C

실험 절차

To a solution of 6-bromo-2-chloro-N-methyl-4-nitropyridin-3-amine 2.59 (1 g, 3.75 mmol) in ethanol (10 ml) was added Fe powder (1.05 g, 18.7 mmol) and a solution of ammonium chloride (1 g, 18.8 mmol) in water (3 mL). The mixture was heated in microwave at 140° C. for 30 min. The mixture was then diluted with EtOAc, filtered and evaporated to give 6-bromo-2-chloro-N3-methylpyridine-3,4-diamine 2.59-A, which was used in the next step without purification.

후처리

  1. filtrationfiltered
  2. customevaporated

출처 및 근거

ORD 기록
ord-2501c82646ee494491e5bc533971e776
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09376441B2

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