Chlorosuccinimide → 3-Chloro-6-fluoro-[1,2,4]triazolo[4,3-a]pyridine

HRID 630723ノート

反応式

HRID 630723 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]([CH:8]=[N:9][N:10]=2)[CH:7]=1.[Cl:11]N1C(=O)CCC1=O>C(Cl)(Cl)Cl>[Cl:11][C:8]1[N:6]2[CH:7]=[C:2]([F:1])[CH:3]=[CH:4][C:5]2=[N:10][N:9]=1

参加物

4

反応物 2

HCID 31398ChlorosuccinimideHCID 552672456-Fluoro-[1,2,4]triazolo[4,3-a]pyridine

生成物 1

HCID 552675403-Chloro-6-fluoro-[1,2,4]triazolo[4,3-a]pyridine収率 76%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A solution of Intermediate 24a (789 mg, 5.98 mmol) and N-chlorosuccinimide (878 mg, 6.57 mmol) in chloroform (15 mL) was heated at 65° C. overnight. The cooled mixture was washed with sat. aq. NaHCO3 solution (2×15 mL) and dried (Na2SO4). The solvent was evaporated, then the residue suspended in diethyl ether (10 mL) and filtered to give the title compound (730 mg, 76%). LCMS (Method 1): Rt 1.83 min, m/z 172 [MH+].

後処理

  1. washThe cooled mixture was washed with sat. aq. NaHCO3 solution (2×15 mL)
  2. dry with materialdried (Na2SO4)
  3. customThe solvent was evaporated
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-35663f74f5f44670bdaa2e233fd9931c
出典データセット
uspto-grants-2016_04
特許番号
US09315503B2

反応ノート

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