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

HRID 1383342
ノート
印刷プレビュー

反応式

HRID 1383342 の反応式
[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]
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 2723922Sodium ethoxideHCID 41710565-Chloro-6-(chloromethyl)-1,2,3,4-tetrahydropyrimidine-2,4-dioneHCID 178507686HCID 178507686、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-b913602ec2df466d9c8f169a2370dbed
出典データセット
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06255314B1

反応ノート

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