Dimethylformamide → HCID 53396122、化合物

HRID 552266

反応式

HRID 552266 の反応式
CN([CH:4]=[O:5])C.O=P(Cl)(Cl)[Cl:8].[F:11][C:12]([F:23])([F:22])[C:13](=O)[CH2:14][C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>O>[Cl:8][C:13]([C:12]([F:23])([F:22])[F:11])=[C:14]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)[CH:4]=[O:5]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 2229581,1,1-Trifluoro-3-phenyl-2-propanone

生成物 1

HCID 53396122HCID 53396122、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
45 °C

実験手順

At 0° C., DMF (4.3 mL) is carefully treated with phosphoroxychloride (2.8 mL) and the mixture is stirred at rt for 20 min before 1,1,1-trifluoro-3-phenyl-propan-2-one (1.55 mL, 10 mmol) is slowly added. The reaction mixture is stirred for 2 h at 45° C. and 18 h at rt, diluted with sat. aq. Na-acetate solution (20 mL) and water (40 mL) and extracted with diethyl ether. The organic phase is separated, washed with sat. aq. NaHCO3-solution, dried over Na2SO4 and evaporated to give 3-chloro-4,4,4-trifluoro-2-phenyl-but-2-enal (2.20 g) as a pale yellow oil.

後処理

  1. additionis slowly added
  2. extractionextracted with diethyl ether
  3. customThe organic phase is separated
  4. washwashed with sat. aq. NaHCO3-solution
  5. dry with materialdried over Na2SO4
  6. customevaporated

出典と根拠

ORDレコード
ord-d4493b7e88f2447ab65b7d7c1a38a2a3
出典データセット
uspto-grants-2011_05
特許番号
US07951794B2

関連ノート

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