Hydrochloric Acid → cis-4-Hydroxy-3-methyl-cyclohexanone

HRID 1028204ノート

反応式

HRID 1028204 の反応式
Cl.[CH3:2][C@H:3]1[C@@H:12]([OH:13])[CH2:11][CH2:10][C:5]2(OCC[O:6]2)[CH2:4]1>CC(C)=O>[OH:13][C@H:12]1[CH2:11][CH2:10][C:5](=[O:6])[CH2:4][C@H:3]1[CH3:2]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 13378641cis-7-Methyl-1,4-dioxa-spiro[4.5]decan-8-ol

生成物 1

HCID 14108184cis-4-Hydroxy-3-methyl-cyclohexanone収率 97.2%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A 1 N hydrochloric acid (250 mL)/acetone (250 mL) mixed solution of cis-7-methyl-1,4-dioxa-spiro[4.5]-decan-8-ol (19.9 g) obtained in Example (14a) was stirred at room temperature for 16 hours. The organic solvent was removed under reduced pressure. The remaining aqueous mixture was subjected to 6 extractions with ethyl acetate. The organic layer was washed with saturated brine, then dried over sodium sulfate, and then concentrated. The residue was dried under reduced pressure to obtain the title compound (14.4 g, 97%) as a colorless oil.

後処理

  1. customThe organic solvent was removed under reduced pressure
  2. extractionThe remaining aqueous mixture was subjected to 6 extractions with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was dried under reduced pressure

出典と根拠

ORDレコード
ord-826517c9cd844f78980558f187dad1d9
出典データセット
uspto-grants-2014_05
特許番号
US08735425B2

反応ノート

読み込み中…