Methylurea → 1-Methylimidazolidine-2,4,5-trione

HRID 76333

反応式

HRID 76333 の反応式
[CH3:1][NH:2][C:3]([NH2:5])=[O:4].[C:6](Cl)(=[O:10])[C:7](Cl)=[O:8]>O1CCCC1.O>[CH3:1][N:2]1[C:7](=[O:8])[C:6](=[O:10])[NH:5][C:3]1=[O:4]

参加物

5

反応物 2

HCID 11719MethylureaHCID 65578Oxalyl chloride

生成物 1

HCID 1231961-Methylimidazolidine-2,4,5-trione収率 94.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To an ice-cold solution of 1-methylurea (200 mg, 2.70 mmol) in dry tetrahydrofuran (6 mL) was added oxalyl chloride (0.26 mL, 2.97 mmol) dropwise, under a nitrogen atmosphere. The reaction mixture was stirred at 0-5° for 2 h and then allowed to warm to room temperature for 1 h before being diluted with water. The product was extracted with ethyl acetate, and the extracts were washed with water, dried and evaporated to give the product as an off-white solid (326 mg, 94%), mp 146-149° C. (lit. 145-148° C.).

後処理

  1. extractionThe product was extracted with ethyl acetate
  2. washthe extracts were washed with water
  3. customdried
  4. customevaporated

出典と根拠

ORDレコード
ord-5270f0fd388c4422b4413078322e13df
出典データセット
uspto-grants-2014_09
特許番号
US08835629B2

関連ノート

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