Hydrochloric Acid → 4-Hydroxy-4-(pyridin-2-yl)cyclohexanone

HRID 549937ノート

反応式

HRID 549937 の反応式
[N:1]1[CH:6]=[CH:5][CH:4]=[CH:3][C:2]=1[C:7]1([OH:17])[CH2:16][CH2:15][C:10]2(OCC[O:11]2)[CH2:9][CH2:8]1.Cl>O1CCCC1>[OH:17][C:7]1([C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][N:1]=2)[CH2:8][CH2:9][C:10](=[O:11])[CH2:15][CH2:16]1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21187637HCID 21187637、化合物

生成物 1

HCID 211876304-Hydroxy-4-(pyridin-2-yl)cyclohexanone収率 92%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

8-Pyridin-2-yl-1,4-dioxaspiro[4.5]decan-8-ol (1.44 g) was dissolved in tetrahydrofuran (25 ml). 2M hydrochloric acid (25 ml) was added and the solution stirred at room temperature overnight. The THF was removed in vacuo and remaining solution made basic with 2M aqueous sodium hydroxide and partitioned with dichloromethane (2×100 ml). Combined organics were dried (sodium sulphate) and concentrated in vacuo to give 4-hydroxy-4-pyridin-2-ylcyclohexanone as an off-white solid (1.07 g, 92%).

後処理

  1. customThe THF was removed in vacuo
  2. custompartitioned with dichloromethane (2×100 ml)
  3. dry with materialCombined organics were dried (sodium sulphate)
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-00c0530ef2164911b874a2af9b83bfa2
出典データセット
uspto-grants-2011_05
特許番号
US07943768B2

反応ノート

読み込み中…