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

HRID 1409743ノート

反応式

HRID 1409743 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

8-(5-Chloropyrimidin-2-yl)-1,4-dioxa-8-azaspiro[4.5]decane (4.2 g) is dissolved in 6 M HCl (50 mL) and stirred at r.t. for 60 h. The solution is cooled in an ice bath and 4 M NaOH (90 mL) is added in portions to make the solution strongly basic (pH ˜14). The mixture is extracted with dichloroemethane (2×200 mL) and the combined dichloromethane layers are dried over Na2SO4, filtered and concentrated to yield the title compound. LC (method 21): tR=4.21 min; Mass spectrum (APCI): m/z=212 [M+H]+.

後処理

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

出典と根拠

ORDレコード
ord-1bbf95e26f614e6390577e9b2a959ce5
出典データセット
uspto-grants-2014_12
特許番号
US08921398B2

反応ノート

読み込み中…