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Potassium Carbonate → 1-(4-Bromo-benzyl)-3-cyclobutylmethyl-imidazolidine-2,4-dione

HRID 2423060
ノート
印刷プレビュー

反応式

HRID 2423060 の反応式
[Br:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][N:7]2[CH2:11][C:10](=[O:12])[NH:9][C:8]2=[O:13])=[CH:4][CH:3]=1.Br[CH2:17][CH:18]1[CH2:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[Br:1][C:2]1[CH:15]=[CH:14][C:5]([CH2:6][N:7]2[CH2:11][C:10](=[O:12])[N:9]([CH2:17][CH:18]3[CH2:21][CH2:20][CH2:19]3)[C:8]2=[O:13])=[CH:4][CH:3]=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 11430Potassium CarbonateHCID 2734658(Bromomethyl)cyclobutaneHCID 154067221-(4-Bromobenzyl)imidazolidine-2,4-dione

生成物 1

HCID 668136401-(4-Bromo-benzyl)-3-cyclobutylmethyl-imidazolidine-2,4-dione収率 71.6%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

i)—To a solution of 1-(4-bromo-benzyl)imidazolidine-2,4-dione (Example 4, step iii) (5.91 g, 21.96 mmol) in DMF (50 ml) were added (bromomethyl)cyclobutane (6.55 g, 43.9 mmol) and potassium carbonate (9.11 g, 65.9 mmol) under a nitrogen atmosphere. After stirring for 20 h at room temperature, the reaction mixture was concentrated under reduced pressure. The product was extracted in ethyl acetate and the combined organic layers were washed with water, brine, dried over sodium sulfate and concentrated under reduced pressure to give 1-(4-bromo-benzyl)-3-cyclobutylmethyl-imidazolidine-2,4-dione (5.30 g).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. extractionThe product was extracted in ethyl acetate
  3. washthe combined organic layers were washed with water, brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-f13ae18389c542a1a66eeaf04c58b0c4
出典データセット
uspto-grants-2011_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07960560B2

反応ノート

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