Triethylamine → HCID 66585107, 화합물

HRID 1630017노트

반응식

HRID 1630017 반응식
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

참가 물질

5

반응물 3

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

생성물 1

HCID 66585107HCID 66585107, 화합물수율 103.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5658ae82a0694839be93a022ea560653
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08791119B2

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