Sodium Hydroxide → 1-(5-Chloropyrimidin-2-yl)piperidin-4-one

HRID 68793ノート

反応式

HRID 68793 の反応式
[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:17][CH2:16][C:11]3(OCC[O:12]3)[CH2:10][CH2:9]2)=[N:6][CH:7]=1.[OH-].[Na+]>Cl>[Cl:1][C:2]1[CH:3]=[N:4][C:5]([N:8]2[CH2:17][CH2:16][C:11](=[O:12])[CH2:10][CH2:9]2)=[N:6][CH:7]=1

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 682901798-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane

生成物 1

HCID 682896071-(5-Chloropyrimidin-2-yl)piperidin-4-one

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

A solution of 8-(5-chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane (4.2 g) in 6 M aqueous HCl (50 mL) is stirred at room temperature for 60 h. The solution is cooled in ice bath and 4 M aqueous NaOH solution (90 mL) is added in portions to make the solution strongly basic (pH˜14). The mixture is extracted with dichloromethane (2×200 mL) and the combined organic layers are dried over Na2SO4, filtered and concentrated to yield the title compound.

後処理

  1. temperatureThe solution is cooled in ice bath
  2. extractionThe mixture is extracted with dichloromethane (2×200 mL)
  3. dry with materialthe combined organic layers are dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-d9c085edf15e415ebd1c4247be5d2954
出典データセット
uspto-grants-2014_09
特許番号
US08822471B2

反応ノート

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