1-Phenylpiperazine → HCID 58484341, 화합물

HRID 42702

반응식

HRID 42702 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 58484341HCID 58484341, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-3688fac5655641648d7b461d2baad2b5
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08536210B2

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