Sulfuric Acid → Carbamimidic acid, methyl ester, sulfate (1:1)

HRID 496832

反応式

HRID 496832 の反応式
[S:1](=[O:5])(=[O:4])([OH:3])[OH:2].[N:6]#[C:7][NH2:8].[CH3:9][OH:10].OS(O)(=O)=O>CO>[S:1]([OH:5])([OH:4])(=[O:3])=[O:2].[CH3:9][O:10][C:7](=[NH:8])[NH2:6]

参加物

5

反応物 3

HCID 1118Sulfuric AcidHCID 9864CyanamideHCID 18363649Sulfuric acid methanol

生成物 1

HCID 169039Carbamimidic acid, methyl ester, sulfate (1:1)

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

Sulfuric acid (112.7 g, 0.97 mol) was added carefully to a cooled CH3OH (150 mL) solution. In a separate flask, cyanamide (50 g, 1.19 mol) was dissolved in methanol (100 mL) and chilled to ca 5° C. in ice-water. Over 2 h, the MeOH—H2SO4 solution was added such that the reaction temperature did not rise above 10° C. After the last addition, the solution was stirred for an additional 1 h and then concentrated in vacuo to give O-methylisourea hydrogen sulfate as a thick-viscous syrup with an assumed quantitative yield which was used directly in the next step.

後処理

  1. customdid not rise above 10° C
  2. additionAfter the last addition
  3. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9c15bd351ced45598ef3bae1efabebcd
出典データセット
uspto-grants-2005_09
特許番号
US06946554B2

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