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Sodium ethoxide → 5-Chloro-6-(1-(2-iminopyrrolidinyl) methyl)uracil hydrochloride

HRID 1383342
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HRID 1383342 반응식
[Cl:1][C:2]1[C:3](=[O:11])[NH:4][C:5](=[O:10])[NH:6][C:7]=1[CH2:8]Cl.[NH:12]=[C:13]1[CH2:17][CH2:16][CH2:15][NH:14]1.[O-]CC.[Na+]>CN(C)C=O>[ClH:1].[Cl:1][C:2]1[C:3](=[O:11])[NH:4][C:5](=[O:10])[NH:6][C:7]=1[CH2:8][N:14]1[CH2:15][CH2:16][CH2:17][C:13]1=[NH:12]
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참가 물질

5

반응물 3

HCID 2723922Sodium ethoxideHCID 41710565-Chloro-6-(chloromethyl)-1,2,3,4-tetrahydropyrimidine-2,4-dioneHCID 178507686HCID 178507686, 화합물

생성물 1

HCID 99037785-Chloro-6-(1-(2-iminopyrrolidinyl) methyl)uracil hydrochloride수율 74.9%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 5.0 g of 5-chloro-6-chloromethyluracil, 6.14 g of 2-iminopyrrolidine and 5.24 g of sodium ethoxide in N,N-dimethylformamide (50 ml) was stirred at room temperature for 14 hours. A crystallized matter was collected by filtration and then suspended in 30 ml of water. After the suspension was neutralized with acetic acid and then washed, an insoluble matter was collected by filtration and then dissolved in 60 ml of 1 N hydrochloric acid. Activated carbon was added to the resultant solution, followed by filtration. The filtrate was concentrated under reduced pressure, and the residue so obtained was washed with ethanol and collected by filtration, whereby 2.68 g of the title compound were obtained (yield: 38%).

후처리

  1. filtrationA crystallized matter was collected by filtration
  2. washwashed
  3. filtrationan insoluble matter was collected by filtration
  4. dissolutiondissolved in 60 ml of 1 N hydrochloric acid
  5. additionActivated carbon was added to the resultant solution
  6. filtrationfollowed by filtration
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. customthe residue so obtained
  9. washwas washed with ethanol
  10. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-b913602ec2df466d9c8f169a2370dbed
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06255314B1

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