Dimethylformamide dimethyl acetal → 2-[(Dimethylamino)methylene]-5,5-dimethylcyclopentanone

HRID 721983

反応式

HRID 721983 の反応式
CO[CH:3](OC)[N:4]([CH3:6])[CH3:5].[CH3:9][C:10]1([CH3:16])[CH2:14][CH2:13][CH2:12][C:11]1=[O:15]>>[CH3:6][N:4]([CH:3]=[C:12]1[CH2:13][CH2:14][C:10]([CH3:16])([CH3:9])[C:11]1=[O:15])[CH3:5]

参加物

3

反応物 2

HCID 78373Dimethylformamide dimethyl acetalHCID 1382862,2-Dimethylcyclopentanone

生成物 1

HCID 695835902-[(Dimethylamino)methylene]-5,5-dimethylcyclopentanone収率 83%

実験手順

A mixture of N,N-dimethylformamide dimethyl acetal (67 mL, 503 mmol) and 2,2-dimethylcyclopentanone (10 g, 90 mmol) was heated at reflux for 2 days. The reaction mixture was then cooled down to room temperature and concentrated. Water (˜380 mL) was added to the residue, and the resulting solution was extracted with methylene chloride. The organic layer was separated, dried over MgSO4 and concentrated to give the title compound (12.5 g) as a yellow-orange oil.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 2 days
  3. concentrationconcentrated
  4. additionWater (˜380 mL) was added to the residue
  5. extractionthe resulting solution was extracted with methylene chloride
  6. customThe organic layer was separated
  7. dry with materialdried over MgSO4
  8. concentrationconcentrated

出典と根拠

ORDレコード
ord-1228a11e329049219729c13590d0d8db
出典データセット
uspto-grants-2006_11
特許番号
US07138361B2

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