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Dimethylformamide → 4-(2-Cyanoethyl)-5-methyl-2-phenyloxazole

HRID 1294183
ノート
印刷プレビュー

反応式

HRID 1294183 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][CH2:14][C:15]([NH2:17])=O.CN(C)C=O.P(Cl)(Cl)(Cl)=O>O>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][CH2:14][C:15]#[N:17]
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 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 178613843-(5-Methyl-2-phenyl-4-oxazolyl)propanamide

生成物 1

HCID 120932634-(2-Cyanoethyl)-5-methyl-2-phenyloxazole収率 89%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a mixture of 3-(5-methyl-2-phenyl-4-oxazolyl)propanamide (5.0 g) and N,N-dimethylformamide (100 ml) was added phosphoryl chloride (3.33 g) at room temperature and the mixture was stirred at room temperature for 1 hr. To the reaction mixture was added water and the mixture was extracted with ethyl acetate. The organic layer was washed successively with water and saturated brine, dried over anhydrous magnesium sulfate, and concentrated to give crystals (4.10 g, 89%) of 3-(5-methyl-2-phenyl-4-oxazolyl)propionitrile. Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 63-64° C.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed successively with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-3b2e52956fe2447b9bbf38beea6e5d9f
出典データセット
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07238716B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート