Triethylamine → HCID 66585107、化合物

HRID 1630017ノート

反応式

HRID 1630017 の反応式
Cl.[N:2]1([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:7][CH2:6][NH:5][CH:4]([C:8]([O:10][CH3:11])=[O:9])[CH2:3]1.C(N(CC)CC)C.[CH:26]1([C:29](Cl)=[O:30])[CH2:28][CH2:27]1>ClCCl>[CH:26]1([C:29]([N:5]2[CH2:6][CH2:7][N:2]([C:12]([O:14][C:15]([CH3:18])([CH3:17])[CH3:16])=[O:13])[CH2:3][CH:4]2[C:8]([O:10][CH3:11])=[O:9])=[O:30])[CH2:28][CH2:27]1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 77637Cyclopropanecarbonyl chlorideHCID 450721861-Tert-butyl 3-methyl piperazine-1,3-dicarboxylate hydrochloride

生成物 1

HCID 66585107HCID 66585107、化合物収率 103.4%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution cooled to 0° C. of 10.0 g (35.6 mmol) of 1-tert-butyl 3-methyl piperazine-1,3-dicarboxylate hydrochloride (CAS 129799-08-2) in 350 ml of dichloromethane are added 11.0 ml (79.1 mmol) of triethylamine and then, over 35 minutes, 3.6 ml (40 mmol) of cyclopropylcarbonyl chloride dissolved in 50 ml of dichloromethane. The medium is stirred from 0° C. to room temperature over 4 hours 30 minutes and is then washed with twice 40 ml of water and dried over sodium sulfate. The solvent is evaporated off under reduced pressure and the residue is chromatographed on a column of 90 g of silica gel, eluting with a mixture of 5 to 50% ethyl acetate in dichloromethane, to give 11.5 g 1-tert-butyl 3-methyl 4-cyclopropanecarbonylpiperazine-1,3-dicarboxylate in the form of a viscous oil.

後処理

  1. washis then washed with twice 40 ml of water
  2. dry with materialdried over sodium sulfate
  3. customThe solvent is evaporated off under reduced pressure
  4. customthe residue is chromatographed on a column of 90 g of silica gel
  5. washeluting with a mixture of 5 to 50% ethyl acetate in dichloromethane

出典と根拠

ORDレコード
ord-5658ae82a0694839be93a022ea560653
出典データセット
uspto-grants-2014_07
特許番号
US08791119B2

反応ノート

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