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Water → 4-(2-Trifluoromethylphenyl)-3-buten-2-one

HRID 9927
ノート
印刷プレビュー

反応式

HRID 9927 の反応式
CON(C)[C:4](=[O:17])[CH:5]=[CH:6][C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][C:8]=1[C:13]([F:16])([F:15])[F:14].C[Li].O.[C:22](OCC)(=O)C>O1CCCC1.C(OCC)C>[F:14][C:13]([F:16])([F:15])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=1[CH:6]=[CH:5][C:4](=[O:17])[CH3:22]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 73858026N-methoxy-N-methyl-3-(2-trifluoromethylphenyl)acrylamideHCID 178418348HCID 178418348、化合物

生成物 1

HCID 5226124-(2-Trifluoromethylphenyl)-3-buten-2-one

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒
HCID 8028
Tetrahydrofuran
溶媒

反応条件

温度
-78 °C

実験手順

11 g of N-methoxy-N-methyl-3-(2-trifluoromethylphenyl)acrylamide are dissolved in 150 ml of dry tetrahydrofuran under a nitrogen atmosphere, cooled to −78° C. and treated dropwise with 36 ml of a 1.4N solution of methyllithium in diethyl ether in 10 minutes. The solution is subsequently furthermore stirred at −78° C. for 2 h and then hydrolysed with water. 200 ml of ethyl acetate are now added at ambient temperature and the mixture is washed three times with saturated sodium chloride solution. The organic phase is finally separated, dried with magnesium sulfate and evaporated under reduced pressure. After purifying by flash chromatography, the title compound is thus obtained.

後処理

  1. washthe mixture is washed three times with saturated sodium chloride solution
  2. customThe organic phase is finally separated
  3. dry with materialdried with magnesium sulfate
  4. customevaporated under reduced pressure
  5. customAfter purifying by flash chromatography

出典と根拠

ORDレコード
ord-b59c10a751ce41438cf1eb1cd9957f87
出典データセット
uspto-grants-2006_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07091371B2

反応ノート

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