Ethyl Acetate → 2-Dimethylamino-4-(naphth-1-yl)oxazole

HRID 33562

反応式

HRID 33562 の反応式
Br[CH2:2][C:3]([C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=2)[CH:8]=[CH:7][CH:6]=1)=O.[CH3:15][N:16]([CH3:20])[C:17]([NH2:19])=[O:18].C(OCC)(=O)C>CN(C)C=O>[CH3:15][N:16]([CH3:20])[C:17]1[O:18][CH:2]=[C:3]([C:5]2[C:14]3[C:9](=[CH:10][CH:11]=[CH:12][CH:13]=3)[CH:8]=[CH:7][CH:6]=2)[N:19]=1

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 11737N,N-DimethylureaHCID 38305132-Bromo-1-(1-naphthalenyl)ethanone

生成物 1

HCID 597968722-Dimethylamino-4-(naphth-1-yl)oxazole

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

1-(α-Bromoacetyl)naphthalene (5 g) and 1,1-dimethylurea (6 g) were stirred in anhydrous dimethylformamide (20 ml) at 105° C. overnight. The mixture was cooled, added to ethyl acetate, washed with sodium bicarbonate solution, water, brine, dried with sodium sulphate, filtered and evaporated in vacuo. The title compound was obtained (0.60 g; m.p. 30-32° C.) following silica gel column chromatography of the residue in dichloromethane.

後処理

  1. temperatureThe mixture was cooled
  2. washwashed with sodium bicarbonate solution, water, brine
  3. dry with materialdried with sodium sulphate
  4. filtrationfiltered
  5. customevaporated in vacuo

出典と根拠

ORDレコード
ord-31fee4816a474d2a8db741e1ab749da3
出典データセット
uspto-grants-2008_09
特許番号
US07429607B2

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