Piperidine → HCID 68537123, 화합물

HRID 1931408노트

반응식

HRID 1931408 반응식
[H-].[Na+].[NH:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1.C([O:11][C:12](=O)[CH2:13][C:14]([CH3:31])([C:16]1[N:17]=[C:18]([C:21]2[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=2)[S:19][CH:20]=1)[CH3:15])C>CN(C=O)C>[CH3:31][C:14]([C:16]1[N:17]=[C:18]([C:21]2[CH:22]=[CH:23][C:24]([C:27]([F:29])([F:30])[F:28])=[CH:25][CH:26]=2)[S:19][CH:20]=1)([CH3:15])[CH2:13][C:12]([N:3]1[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)=[O:11]

참가 물질

5

반응물 3

HCID 8082PiperidineHCID 24758Sodium hydrideHCID 68537700HCID 68537700, 화합물

생성물 1

HCID 68537123HCID 68537123, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

27.5 mg (0.63 mmol) of sodium hydride (55% in mineral oil) were added to 53.6 mg (0.63 mmol) of piperidine in 2 ml of DMF. After stirring at room temperature for 30 min, 150 mg (0.42 mmol) of 3-methyl-3-[2-(4-trifluoromethyl-phenyl)-thiazol-4-yl]-butyric acid ethyl ester in 2 ml of DMF were added, and the reaction mixture was stirred at room temperature for 2 h. After evaporation, water and dichloromethane were added, the organic phase was separated, washed with water, dried, and evaporated. The product was purified by RP18 chromatography. Yield: 6.3 mg.

후처리

  1. stirringthe reaction mixture was stirred at room temperature for 2 h
  2. customAfter evaporation, water and dichloromethane
  3. additionwere added
  4. customthe organic phase was separated
  5. washwashed with water
  6. customdried
  7. customevaporated
  8. customThe product was purified by RP18 chromatography

출처 및 근거

ORD 기록
ord-1906d63586d14b4c88ae3b122a0329d3
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188291B2

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