Urea → 5-Methylbenzimidazol-2-one

HRID 2233532

反応式

HRID 2233532 の反応式
[NH2:1][C:2]([NH2:4])=[O:3].N[C:6]1[CH:7]=[C:8]([CH3:13])[CH:9]=[CH:10][C:11]=1N>C(O)CCCC>[CH3:13][C:8]1[CH:7]=[CH:6][C:11]2=[N:1][C:2](=[O:3])[N:4]=[C:10]2[CH:9]=1

参加物

4

反応物 2

HCID 1176UreaHCID 103323,4-Diaminotoluene

生成物 1

HCID 200643865-Methylbenzimidazol-2-one収率 56%

試薬・触媒・溶媒 1

HCID 62761-Pentanol溶媒

実験手順

A solution of urea (6.00 g, 0.1000 mol) and 3,4-diaminotoluene (1) (12.20 g, 0.0999 mol) in pentan-1-ol (40 mL) was vigorously stirred and heated to reflux under a nitrogen atmosphere. After 2 hours the heating was discontinued and on cooling to room temperature a pink solid settled out. This was filtered off and recrystallised from boiling ethanol (17.98 g. in 400 mL) to give 2 crops of 5-methylbenzimidazol-2-one (2) as a pink powder. The total mass was recovered was 8.21 g (56% yield);

後処理

  1. temperatureheated
  2. temperatureto reflux under a nitrogen atmosphere
  3. filtrationThis was filtered off
  4. customrecrystallised

出典と根拠

ORDレコード
ord-16d89af2f50a46ddb6d07647829ab2f9
出典データセット
uspto-grants-2010_05
特許番号
US07709514B2

関連ノート

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