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Water → N2-Methylpyridine-2,6-diamine

HRID 1014113
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HRID 1014113 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH2:8])[N:3]=1.[C:9]([O-])([O-])=O.[K+].[K+].CI.O>C1COCC1>[CH3:9][NH:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([NH2:8])[N:3]=1
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참가 물질

6

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 88612,6-DiaminopyridineHCID 11430Potassium Carbonate

생성물 1

HCID 55281082N2-Methylpyridine-2,6-diamine수율 10%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 2,6-diaminopyridine (10 g, 91.63 mmol) in dry THF (100 mL) was added K2CO3 (18.8 g, 136.23 mmol) and CH3I (13 g, 91.63 mmol) and the reaction mixture was stirred at room temperature for 16 h. Water was added (10 mL) and the mixture was extracted with EtOAc (100 mL). The EtOAc layer was dried and was concentrated under reduced pressure. The residue was further purified by column chromatography (SiO2, 60-120, chloroform) to give 2-methylamino-6-aminopyridine (1.1 g, 10%) as a brown solid.

후처리

  1. extractionthe mixture was extracted with EtOAc (100 mL)
  2. dry with materialThe EtOAc layer was dried
  3. concentrationwas concentrated under reduced pressure
  4. customThe residue was further purified by column chromatography (SiO2, 60-120, chloroform)

출처 및 근거

ORD 기록
ord-bdd68b501c7a44a1b4f3e0f0ea013f9f
출처 데이터셋
uspto-grants-2011_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07982036B2

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