2-Boc-Amino-3-iodo-4-chloropyridine → 4-Chloro-3-iodopyridin-2-amine

HRID 919299ノート

反応式

HRID 919299 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH:8]C(=O)OC(C)(C)C)[C:3]=1[I:16]>Br>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:16]

参加物

3

反応物 1

HCID 598528862-Boc-Amino-3-iodo-4-chloropyridine

生成物 1

HCID 229365964-Chloro-3-iodopyridin-2-amine

試薬・触媒・溶媒 1

HCID 260Hydrogen Bromide溶媒

反応条件

温度
100 °C

実験手順

The solution of tert-butyl 4-chloro-3-iodopyridin-2-ylcarbamate (3.2 g, 9 mmol) in HBr (48%, 15 mL) was allowed to stir at 100° C. for 1 h. The reaction mixture was concentrated and the resulting residue was neutralized with aqueous Na2CO3, extracted with EtOAc (2×25 mL), dried over Na2SO4, filtered and concentrated to used in next step directly without further purification. LC/MS m/z=255.19 [M+H]+

後処理

  1. concentrationThe reaction mixture was concentrated
  2. extractionextracted with EtOAc (2×25 mL)
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated
  6. customto used in next step directly without further purification

出典と根拠

ORDレコード
ord-8fddd853c3c747f1be988788d1a28ff7
出典データセット
uspto-grants-2016_03
特許番号
US09273033B2

反応ノート

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