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

HRID 1358227
ノート
印刷プレビュー

反応式

HRID 1358227 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-imino pyrrolidine and 5.24 g of sodium ethoxide in 50 ml of N,N-dimethylformamide was stirred at room temperature for 14 hours. The resulting crystals were collected by filtration and suspended in 30 ml of water. The suspension was neutralized with acetic acid and washed. The insoluble substances were collected by filtration and dissolved in 60 ml of 1N hydrochloric acid. After addition of activated carbon, the resulting mixture was filtered. The filtrate was concentrated under reduced pressure and the residue was washed with ethanol and collected by filtration, giving 2.68 g of the desired compound (yield 38%). The physical properties of this compound are as follows:

後処理

  1. filtrationThe resulting crystals were collected by filtration
  2. washwashed
  3. filtrationThe insoluble substances were collected by filtration
  4. dissolutiondissolved in 60 ml of 1N hydrochloric acid
  5. additionAfter addition of activated carbon
  6. filtrationthe resulting mixture was filtered
  7. concentrationThe filtrate was concentrated under reduced pressure
  8. washthe residue was washed with ethanol
  9. filtrationcollected by filtration

出典と根拠

ORDレコード
ord-0be4a01814f343d78cd2737a0230425c
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06596720B1

反応ノート

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