Sodium Carbonate → N-(3-Trifluoromethyl-phenyl)-N'-propargyl-piperazine hydrochloride

HRID 255877ノート

反応式

HRID 255877 の反応式
Cl.[F:2][C:3]([F:17])([F:16])[C:4]1[CH:5]=[C:6]([N:10]2[CH2:15][CH2:14][NH:13][CH2:12][CH2:11]2)[CH:7]=[CH:8][CH:9]=1.[CH2:18]([Cl:21])[C:19]#[CH:20].C(=O)([O-])[O-].[Na+].[Na+]>C(#N)C>[ClH:21].[F:17][C:3]([F:2])([F:16])[C:4]1[CH:5]=[C:6]([N:10]2[CH2:15][CH2:14][N:13]([CH2:20][C:19]#[CH:18])[CH2:12][CH2:11]2)[CH:7]=[CH:8][CH:9]=1

参加物

5

反応物 3

HCID 10340Sodium Carbonate2 回HCID 122213-Chloro-1-propyne2 回HCID 3084246TFMPP hydrochloride

生成物 1

HCID 13116712N-(3-Trifluoromethyl-phenyl)-N'-propargyl-piperazine hydrochloride

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

3.2 g (0.012 mol) of N-(3-trifluoromethyl-phenyl)-piperazine hydrochloride, 0.9 g (0.012 mol) of propargyl chloride and 2.5 g (0.024 mol) of sodium carbonate were heated at 60° C. in 50 ml of absolute acetonitrile while stirring. Over a period of 15 hours, an additional 0.34 g (0.0046 mol) of propargyl chloride and 0.5 g (0.0046 mol) of sodium carbonate were added. The inorganic salts were removed by suction filtration, and the filtrate was evaporated under reduced pressure. The evaporation residue was dissolved in toluene, and the product solution was extracted with the calculated quantity of dilute hydrochloric acid. The aqueous phase was made alkaline with soda, and the base was extracted with ether. After drying with sodium sulfate, the organice phase was evaporated under reduced pressure, and the base was converted into its hydrochloride in conventional manner. White crystals from acetonitrile, melting point 218°-219° C. (decomposition). Yield: 2.7 g (73.8% of theory). The existence of these compounds was confirmed by elemental and spectrum analysis.

後処理

  1. customThe inorganic salts were removed by suction filtration
  2. customthe filtrate was evaporated under reduced pressure
  3. dissolutionThe evaporation residue was dissolved in toluene
  4. extractionthe product solution was extracted with the calculated quantity of dilute hydrochloric acid
  5. extractionthe base was extracted with ether
  6. dry with materialAfter drying with sodium sulfate
  7. customthe organice phase was evaporated under reduced pressure

出典と根拠

ORDレコード
ord-d4343479822d4030b7c098531a0b7fe7
出典データセット
uspto-grants-1987_10
特許番号
US04699910

反応ノート

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