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Triethylamine → HCID 66598990、化合物

HRID 1889003
ノート
印刷プレビュー

反応式

HRID 1889003 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

HCID 66598990HCID 66598990、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1f202b39dd454cc2b182d35a5462ad63
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08501946B2

反応ノート

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