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Guanidine Hydrochloride → Methyl 2-amino-1,6-dihydro-6-oxo-4-pyrimidinecarbamate

HRID 464782
ノート
印刷プレビュー

反応式

HRID 464782 の反応式
[Na].Cl.[NH2:3][C:4]([NH2:6])=[NH:5].[CH3:7][O:8][C:9](=[O:21])[N:10]=[CH:11][CH2:12][C:13](OCCOCC)=[O:14]>CO>[NH2:5][C:4]1[NH:6][C:13](=[O:14])[CH:12]=[C:11]([NH:10][C:9]([O:8][CH3:7])=[O:21])[N:3]=1
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 5742Guanidine HydrochlorideHCID 5360545SodiumHCID 86740383Methyl[(1-ethoxy-2-ethoxycarbonyl)ethylidene]carbamate

生成物 1

HCID 135964809Methyl 2-amino-1,6-dihydro-6-oxo-4-pyrimidinecarbamate

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

10 g of sodium are dissolved in 200 ml of absolute methanol, whereupon the solution is treated with 30 g of guanidine hydrochloride. While stirring there is added thereto a solution of 50 g of methyl[(1-ethoxy-2-ethoxycarbonyl)ethylidene]carbamate in 150 ml of absolute methanol. The resulting suspension is stirred overnight and thereafter concentrated at 40° in a water-jet vacuum. 600 ml of water are added to the residue and the resulting suspension is adjusted to pH 5 with glacial acetic acid while stirring. The resulting precipitate is filtered off under suction, washed with 250 ml of water and dried at 50° in vacuo. There is obtained methyl 2-amino-1,6-dihydro-6-oxo-4-pyrimidinecarbamate which is uniform according to thin-layer chromatography.

後処理

  1. additionis added
  2. stirringThe resulting suspension is stirred overnight
  3. concentrationconcentrated at 40° in a water-jet vacuum
  4. addition600 ml of water are added to the residue
  5. stirringwhile stirring
  6. filtrationThe resulting precipitate is filtered off under suction
  7. washwashed with 250 ml of water
  8. customdried at 50° in vacuo

出典と根拠

ORDレコード
ord-46c6d67cd0064b398dfc78ebae4bcbd5
出典データセット
uspto-grants-1985_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04549019

反応ノート

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