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Sodium Hydroxide → 6-Iodo-4-methylpyridin-3-amine

HRID 218470
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HRID 218470 반응식
Cl[Sn]Cl.O.[I:5][C:6]1[CH:11]=[C:10]([CH3:12])[C:9]([N+:13]([O-])=O)=[CH:8][N:7]=1.[OH-].[Na+]>CCOC(C)=O>[I:5][C:6]1[CH:11]=[C:10]([CH3:12])[C:9]([NH2:13])=[CH:8][N:7]=1
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참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 230701672-Iodo-4-methyl-5-nitropyridineHCID 43835034Tin dichloride dihydrate

생성물 1

HCID 230701206-Iodo-4-methylpyridin-3-amine수율 99%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매2회

실험 절차

To a solution of SnCl2.H2O (20.5 g, 108 mmol) in EtOAc (200 mL) was added 2-iodo-4-methyl-5-nitropyridine (5.7 g, 21.6 mmol) in EtOAc (20 mL). Heat was released, and the reaction mixture was kept at reflux for 2 hr. After cooling to rt, the reaction mixture was treated with 50% NaOH (50 mL). Solid was filtered off and washed with EtOAc. The filtrate was washed with brine, dried, and concentrated to afford 2-iodo-4-methyl-5-pyridinamine (5 g, 99%) as a yellow solid.

후처리

  1. temperatureHeat
  2. temperatureat reflux for 2 hr
  3. filtrationSolid was filtered off
  4. washwashed with EtOAc
  5. washThe filtrate was washed with brine
  6. customdried
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-bbbbf47f9c13471fbab8bdaeb0ef81e0
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08198456B2

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