Sodium Hydroxide → 2-(2-Chloropyridin-4-yl)-2,4-diazabicyclo[3.1.0]hexan-3-one

HRID 523580ノート

反応式

HRID 523580 の反応式
[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[CH:13]3[CH:11]([CH2:12]3)[N:10](C(OCC3C=CC=CC=3)=O)[C:9]2=[O:24])[CH:5]=[CH:4][N:3]=1.[OH-].[Na+]>Cl>[Cl:1][C:2]1[CH:7]=[C:6]([N:8]2[C:9](=[O:24])[NH:10][CH:11]3[CH:13]2[CH2:12]3)[CH:5]=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 86729664Benzyl 4-(2-chloropyridin-4-yl)-3-oxo-2,4-diazabicyclo[3.1.0]hexane-2-carboxylate

生成物 1

HCID 867296652-(2-Chloropyridin-4-yl)-2,4-diazabicyclo[3.1.0]hexan-3-one収率 83%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of benzyl 4-(2-chloropyridin-4-yl)-3-oxo-2,4-diazabicyclo-[3.1.0]hexane-2-carboxylate (I-30b: 20.0 mg, 0.058 mmol) in 3.0 mL of 6N HCl was heated to 100° C. for 1 hour. The resulting mixture was basified with 1N NaOH. The reaction mixture was cooled and partitioned between ethyl acetate and water. The organic layer was concentrated and washed with hexane to afford 10 mg of the product (83% yield).

後処理

  1. temperatureThe reaction mixture was cooled
  2. custompartitioned between ethyl acetate and water
  3. concentrationThe organic layer was concentrated
  4. washwashed with hexane

出典と根拠

ORDレコード
ord-10369414a844402d92dc6baf6ddd84c9
出典データセット
uspto-grants-2016_05
特許番号
US09339501B2

反応ノート

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