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

HRID 572422ノート

反応式

HRID 572422 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-6c8dc0decbcd4ca8b84e043e6063eb9d
出典データセット
uspto-grants-2015_05
特許番号
US09029399B2

反応ノート

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