Trichloroacetyl chloride → HCID 54546861, 화합물

HRID 1654524

반응식

HRID 1654524 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 54546861HCID 54546861, 화합물

시약·촉매·용매 2

HCID 10290809Zinc copper couple촉매HCID 3283Diethyl Ether용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-f93c6ca023284b8aaa1e21fb81539071
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05407943

연결된 노트

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