Piperidine → HCID 68537123、化合物

HRID 1931408ノート

反応式

HRID 1931408 の反応式
[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]

参加物

5

反応物 3

HCID 8082PiperidineHCID 24758Sodium hydrideHCID 68537700HCID 68537700、化合物

生成物 1

HCID 68537123HCID 68537123、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1906d63586d14b4c88ae3b122a0329d3
出典データセット
uspto-grants-2012_05
特許番号
US08188291B2

反応ノート

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