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Triethylamine → HCID 66598990, 화합물

HRID 1889003
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HRID 1889003 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][C:2]1=[O:7].C(N(CC)CC)C.[Cl:15][C:16]1[CH:24]=[CH:23][C:19]([C:20](Cl)=[O:21])=[C:18]([C:25]([F:28])([F:27])[F:26])[CH:17]=1>ClCCl>[Cl:15][C:16]1[CH:24]=[CH:23][C:19]([C:20]([N:4]2[CH2:5][CH2:6][NH:1][C:2](=[O:7])[CH2:3]2)=[O:21])=[C:18]([C:25]([F:26])([F:27])[F:28])[CH:17]=1
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 231360Piperazin-2-oneHCID 43403694-Chloro-2-(trifluoromethyl)benzoyl chloride

생성물 1

HCID 66598990HCID 66598990, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

2-piperazinone (0.5 g, 4.99 mmol, commercially available from e.g. Sigma-Aldrich) was dissolved in dichloromethane (DCM) (30 mL), and to this was added triethylamine (0.835 mL, 5.99 mmol). The solution was then cooled to 0° C. before 4-chloro-2-(trifluoromethyl)benzoyl chloride (1.335 g, 5.49 mmol, commercially available from e.g. 3B Scientific or APAC) in dichloromethane (DCM) (5 mL) was added dropwise. The solution was stirred, under argon, for 30 minutes before the solvent was evaporated in vacuo. The remaining residue was then dissolved in DCM (20 mL) and the solution was washed with water (10 mL), a saturated solution of sodium bicarbonate (10 mL) and brine (10 mL). The organic phase was then dried over anhydrous sodium sulphate, and the solid sodium sulphate was then filtered off. The solvent was then evaporated in vacuo, and the remaining solid was stirred in hexane, at 55° C., for 30 minutes. The solid was then filtered off to yield the desired product in 1.445 g.

후처리

  1. customwas evaporated in vacuo
  2. dissolutionThe remaining residue was then dissolved in DCM (20 mL)
  3. washthe solution was washed with water (10 mL)
  4. dry with materialThe organic phase was then dried over anhydrous sodium sulphate
  5. filtrationthe solid sodium sulphate was then filtered off
  6. customThe solvent was then evaporated in vacuo
  7. stirringthe remaining solid was stirred in hexane, at 55° C., for 30 minutes
  8. filtrationThe solid was then filtered off

출처 및 근거

ORD 기록
ord-1f202b39dd454cc2b182d35a5462ad63
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08501946B2

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