Sodium Hydroxide → 2-((Dimethylamino)methyl)-1-(3-methoxyphenyl)cyclohexanol

HRID 1296ノート

反応式

HRID 1296 の反応式
Cl.[CH3:2][N:3]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=1)[OH:12])[CH3:4].[OH-].[Na+]>O>[CH3:4][N:3]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][C:7]1([C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([O:19][CH3:20])[CH:14]=1)[OH:12])[CH3:2]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 9971980Cyclohexanol, 2-((dimethylamino)methyl)-1-(3-methoxyphenyl)-, hydrochloride (1:1)

生成物 1

HCID 55232-((Dimethylamino)methyl)-1-(3-methoxyphenyl)cyclohexanol収率 99.9%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

3 kg (10 mole) (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol hydrochloride (1) were suspended in 4800 ml water and treated with 1.6 kg crushed ice. 1300 ml of 36-38% (technical) caustic soda solution were added drop-wise with stirring. The mixture was subsequently extracted with 7000 ml dichloromethane, and was extracted with a further 2000 ml dichloromethane after phase separation. The combined organic phases were dried over sodium sulphate. After removing the solvent by distillation, 2630 g (99% theoretical) of (1RS,2RS)-2-dimethylaminomethyl-1-(3-methoxy-phenyl)-cyclohexanol were obtained as a syrup.

後処理

  1. additiontreated with 1.6 kg
  2. customcrushed ice
  3. extractionThe mixture was subsequently extracted with 7000 ml dichloromethane
  4. extractionwas extracted with a further 2000 ml dichloromethane
  5. customafter phase separation
  6. dry with materialThe combined organic phases were dried over sodium sulphate
  7. customAfter removing the solvent
  8. distillationby distillation

出典と根拠

ORDレコード
ord-822a168440d44234b23b8b29fa23f00d
出典データセット
uspto-grants-1998_03
特許番号
US05723668

反応ノート

読み込み中…