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Dimethyl-(8-phenyl-1,4-dioxa-spiro[4.5]dec-8-ylmethyl)-amine → 4-Dimethylaminomethyl-4-phenylcyclohexanone

HRID 76929
ノート
印刷プレビュー

反応式

HRID 76929 の反応式
[CH3:1][N:2]([CH3:20])[CH2:3][C:4]1([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH2:13][CH2:12][C:7]2(OCC[O:8]2)[CH2:6][CH2:5]1>OS(O)(=O)=O>[CH3:20][N:2]([CH2:3][C:4]1([C:14]2[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=2)[CH2:5][CH2:6][C:7](=[O:8])[CH2:12][CH2:13]1)[CH3:1]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 45026964Dimethyl-(8-phenyl-1,4-dioxa-spiro[4.5]dec-8-ylmethyl)-amine

生成物 1

HCID 686322734-Dimethylaminomethyl-4-phenylcyclohexanone

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

The title compound of step 5 (5.40 g, 19.6 mmol) was dissolved in 5% H2SO4 (300 mL) and stirred for 1 d at RT. The solution was then washed with ether three times and the ether phase discarded. The aqueous phase was made alkaline with 5N NaOH with ice cooling and extracted with dichloromethane three times. The organic phase was washed with a little water, dried over Na2SO4 and concentrated to low volume in a vacuum.

後処理

  1. washThe solution was then washed with ether three times
  2. extractionextracted with dichloromethane three times
  3. washThe organic phase was washed with a little water
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to low volume in a vacuum

出典と根拠

ORDレコード
ord-139fa66645ef4da2beb0df6d962c5f50
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08835689B2

反応ノート

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