Trichloroacetyl chloride → HCID 54546861、化合物

HRID 1654524

反応式

HRID 1654524 の反応式
[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][C:14](=[CH2:17])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl:18][C:19](Cl)([Cl:23])[C:20](Cl)=O.P(Cl)(Cl)(Cl)=[O:26]>CCOCC.[Cu].[Zn]>[CH2:1]([O:8][C:9]([N:11]1[CH2:16][CH2:15][C:14]2([C:19]([Cl:23])([Cl:18])[CH2:20][C:17]2=[O:26])[CH2:13][CH2:12]1)=[O:10])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 6420Trichloroacetyl chlorideHCID 24813Phosphorus oxychlorideHCID 15519136Benzyl 4-methylidenepiperidine-1-carboxylate

生成物 1

HCID 54546861HCID 54546861、化合物

試薬・触媒・溶媒 2

HCID 10290809Zinc copper couple触媒HCID 3283Diethyl Ether溶媒2 回

実験手順

To a stirred solution of 1-benzyloxycarbonyl-4-methylenepiperidine (11.1 g, 49.3 mmol) and zinc-copper couple (95: 5, 7.98 g, 12.2 mmol) in 200 ml of anhydrous ether was added a solution of trichloroacetyl chloride (10.18 ml, 91.2 mmol) and phosphorous oxychloride (8.77 ml, 94.0 mmol) in 50 ml of anhydrous ether. The reaction mixture was refluxed overnight. After cooling to room temperature, the solution was filtered through celite and the filtrate was washed with brine and cold sodium bicarbonate, dried over magnesium sulfate and upon evaporation afforded the title compound as a yellow liquid, 15.3 g (crude).

後処理

  1. temperatureThe reaction mixture was refluxed overnight
  2. filtrationthe solution was filtered through celite
  3. washthe filtrate was washed with brine and cold sodium bicarbonate
  4. dry with materialdried over magnesium sulfate and upon evaporation

出典と根拠

ORDレコード
ord-f93c6ca023284b8aaa1e21fb81539071
出典データセット
uspto-grants-1995_04
特許番号
US05407943

関連ノート

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