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

HRID 1017501
ノート
印刷プレビュー

反応式

HRID 1017501 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

5-Chloro-6-chloromethyluracil (5.0 g), 2-iminopyrrolidine (6.14 g), and sodium ethoxide (5.24 g) were dissolved in N,N-dimethylformamide (50 ml) and the resultant solution was stirred for 14 hours at room temperature. Subsequently, precipitated crystals were collected through filtration, and the crystals were suspended in water (30 ml). The resultant suspension was neutralized with acetic acid and washed. Subsequently, insoluble matter was collected through filtration and was dissolved in 1N HCl (60 ml). Activated carbon was added to the resultant solution and the mixture was subjected to filtration. The filtrate was concentrated under reduced pressure, and the residue was washed with ethanol, followed by filtration, to thereby obtain 2.68 g of the title compound (38% yield).

後処理

  1. customSubsequently, precipitated crystals
  2. filtrationwere collected through filtration
  3. washwashed
  4. filtrationSubsequently, insoluble matter was collected through filtration
  5. dissolutionwas dissolved in 1N HCl (60 ml)
  6. additionActivated carbon was added to the resultant solution
  7. filtrationthe mixture was subjected to filtration
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. washthe residue was washed with ethanol
  10. filtrationfollowed by filtration

出典と根拠

ORDレコード
ord-244ee05fe5d64339b42ff3a29d704f61
出典データセット
uspto-grants-2002_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06479500B1

反応ノート

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