1-Phenylpiperazine → HCID 58484341、化合物

HRID 42702

反応式

HRID 42702 の反応式
Cl[C:2]1[N:7]([CH3:8])[C:6](=[O:9])[N:5]([CH3:10])[C:4](=[O:11])[C:3]=1[CH:12]=[O:13].C(N(CC)CC)C.[C:21]1([N:27]2[CH2:32][CH2:31][NH:30][CH2:29][CH2:28]2)[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>ClCCl>[CH3:8][N:7]1[C:2]([N:30]2[CH2:31][CH2:32][N:27]([C:21]3[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=3)[CH2:28][CH2:29]2)=[C:3]([CH:12]=[O:13])[C:4](=[O:11])[N:5]([CH3:10])[C:6]1=[O:9]

参加物

5

反応物 3

HCID 70961-PhenylpiperazineHCID 8471TriethylamineHCID 3199716-Chloro-5-formyl-1,3-dimethyluracil

生成物 1

HCID 58484341HCID 58484341、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To an ice-cooled, stirred solution of 6-chloro-1,3-dimethyl-2,4-dioxo-1,2,3,4-tetrahydropyrimidine-5-carbaldehyde (0.600 g, 2.96 mmol) and triethyl-amine (0.45 ml, 3.26 mmol) in dichloromethane (20 ml), a solution of N-phenylpiperazine (0.49 ml, 3.26 mmol) in dichloromethane (10 ml) was added dropwise. The resulting suspension was stirred at room temperature until the starting material was consumed (3.5 h, monitored by TLC). Then the reaction mixture was washed with water (3×10 ml), and the organic phase was dried over 20, anhydrous MgSO4. The solvent was evaporated in vacuo, and the brown oily crude product was purified by column chromatography with a mixture of dichloromethane:ethyl acetate (1:1) as the eluent and crystallized from ethanol.

後処理

  1. customwas consumed (3.5 h, monitored by TLC)
  2. washThen the reaction mixture was washed with water (3×10 ml)
  3. dry with materialthe organic phase was dried over 20, anhydrous MgSO4
  4. customThe solvent was evaporated in vacuo
  5. customthe brown oily crude product was purified by column chromatography with a mixture of dichloromethane:ethyl acetate (1:1) as the eluent
  6. customcrystallized from ethanol

出典と根拠

ORDレコード
ord-3688fac5655641648d7b461d2baad2b5
出典データセット
uspto-grants-2013_09
特許番号
US08536210B2

関連ノート

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