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Water → 2-(2-(4,4-Dimethyl-oxazolin-2-yl)-benzoyl)4,6-dimethoxypyrimidine

HRID 1779289
ノート
印刷プレビュー

反応式

HRID 1779289 の反応式
[CH3:1][C:2]1([CH3:25])[CH2:6][O:5][C:4]([C:7]2[CH:24]=[CH:23][CH:22]=[CH:21][C:8]=2[CH:9]([C:11]2[N:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[N:12]=2)Br)=[N:3]1.C([O-])([O-])=[O:27].[Na+].[Na+].O>CS(C)=O>[CH3:1][C:2]1([CH3:25])[CH2:6][O:5][C:4]([C:7]2[CH:24]=[CH:23][CH:22]=[CH:21][C:8]=2[C:9]([C:11]2[N:16]=[C:15]([O:17][CH3:18])[CH:14]=[C:13]([O:19][CH3:20])[N:12]=2)=[O:27])=[N:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 10340Sodium CarbonateHCID 190506432-(2-(4,4-Dimethyl-oxazolin-2-yl)-alpha-bromobenzyl)-4,6-dimethoxy pyrimidine

生成物 1

HCID 190506722-(2-(4,4-Dimethyl-oxazolin-2-yl)-benzoyl)4,6-dimethoxypyrimidine

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

A mixture of 1.2 g of 2-(2-(4,4-dimethyl-oxazolin-2-yl)-α-bromobenzyl)-4,6-dimethoxy-pyrimidine and 2 g of Na2CO3 in 30 ml of DMSO is heated with stirring at 50°-60° C. for 3 hrs. The mixture is poured into 150 ml of water and extracted with toluene. The toluene extract is washed twice with water (2×50 ml) separated and concentrated. The thus obtained gum is chromatographed with 800 ml of 80/20 hexane/ethyl acetate, 500 ml 70/30 hexane/ethyl acetate, 60/40 ml hexane/ethyl acetate (50 ml fractions) fractions 29 to 34 yielded the title compound.

後処理

  1. temperatureis heated
  2. extractionextracted with toluene
  3. extractionThe toluene extract
  4. washis washed twice with water (2×50 ml)
  5. customseparated
  6. concentrationconcentrated
  7. customThe thus obtained gum is chromatographed with 800 ml of 80/20 hexane/ethyl acetate, 500 ml 70/30 hexane/ethyl acetate, 60/40 ml hexane/ethyl acetate (50 ml fractions) fractions 29 to 34

出典と根拠

ORDレコード
ord-0a6d9c78335f415185f58894e37420b2
出典データセット
uspto-grants-1997_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05627138

反応ノート

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