Trifluoroacetic acid → 6-Chloro-4-iodo-N-methylpyridin-3-amine

HRID 340424ノート

反応式

HRID 340424 の反応式
[Cl:1][C:2]1[N:7]=[CH:6][C:5]([N:8](C)[C:9](=O)OC(C)(C)C)=[C:4]([I:17])[CH:3]=1.C(O)(C(F)(F)F)=O>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[CH:6][C:5]([NH:8][CH3:9])=[C:4]([I:17])[CH:3]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 57443399Tert-butyl (6-chloro-4-iodopyridin-3-yl)(methyl)carbamate

生成物 1

HCID 574434006-Chloro-4-iodo-N-methylpyridin-3-amine収率 97.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To the solution of tert-butyl (6-chloro-4-iodopyridin-3-yl)(methyl)carbamate (62.5 g, 0.172 mol) in 500 mL of anhydrous DCM was added 180 mL of TFA. Then the solution was stirred at room temperature for 4 hrs. Concentrated to remove the solvent, and purified by flash chromatography to afford 45.1 g 6-chloro-4-iodo-N-methylpyridin-3-amine as a yellow solid (Yield: 97.3%).

後処理

  1. concentrationConcentrated
  2. customto remove the solvent
  3. custompurified by flash chromatography

出典と根拠

ORDレコード
ord-b2a4e43e580642f4b91b3a107698e91e
出典データセット
uspto-grants-2014_11
特許番号
US08895586B2

反応ノート

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