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Triethylamine → 5-{2-[4-(2-tert-Butyl-4-methylphenyl)piperazin-1-yl]-2-oxoethyl}imidazolidine-2,4-dione

HRID 534982
ノート
印刷プレビュー

反応式

HRID 534982 の反応式
Cl.Cl.[C:3]([C:7]1[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]=1[N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1)([CH3:6])([CH3:5])[CH3:4].[O:20]=[C:21]1[NH:25][CH:24]([CH2:26][C:27](O)=[O:28])[C:23](=[O:30])[NH:22]1.C(N(CC)CC)C.CCN=C=NCCCN(C)C.C1C=CC2N(O)N=NC=2C=1.C([O-])(O)=O.[Na+]>CN(C)C=O>[C:3]([C:7]1[CH:12]=[C:11]([CH3:13])[CH:10]=[CH:9][C:8]=1[N:14]1[CH2:15][CH2:16][N:17]([C:27](=[O:28])[CH2:26][CH:24]2[NH:25][C:21](=[O:20])[NH:22][C:23]2=[O:30])[CH2:18][CH2:19]1)([CH3:6])([CH3:4])[CH3:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 6

HCID 8471TriethylamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 954922,5-Dioxo-1,3-diazolidin-4-ylacetic acidHCID 516892Sodium BicarbonateHCID 667508371-(2-Tert-butyl-4-methylphenyl)piperazine dihydrochloride

生成物 1

HCID 66792767
5-{2-[4-(2-tert-Butyl-4-methylphenyl)piperazin-1-yl]-2-oxoethyl}imidazolidine-2,4-dione
収率 89%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 1-(2-tert-butyl-4-methylphenyl)piperazine dihydrochloride (Reference Example 10, 0.31 g, 1.0 mmol), (2,5-dioxoimidazolidin-4-yl)acetic acid (0.19 g, 1.2 mmol), triethylamine (420 μL, 3.0 mmol), EDCI (0.23 g, 1.2 mmol) and HOBt (0.18 g, 1.2 mmol) in N,N-dimethylformamide (5 mL) was stirred at room temperature for 2 days. The reaction mixture was poured into saturated NaHCO3 solution and extracted with ethyl acetate. The extract was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure to give the title compound (0.33 g, 89%) as a orange solid.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-6eda969acc724286a5005179323c4244
出典データセット
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08853215B2

反応ノート

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