Lithium hydride → HCID 178436207、化合物

HRID 903906ノート

反応式

HRID 903906 の反応式
I.[NH:2]=[C:3]1[NH:7][CH2:6][CH2:5][NH:4]1.[H-].[Li+].[CH2:10]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:13]=1[N:19]=[C:20]=[O:21])[CH3:11]>CN(C)C=O>[CH2:10]([C:12]1[CH:17]=[CH:16][CH:15]=[C:14]([CH3:18])[C:13]=1[NH:19][C:20]([N:2]=[C:3]1[NH:7][CH2:6][CH2:5][NH:4]1)=[O:21])[CH3:11]

参加物

5

反応物 3

HCID 62714Lithium hydrideHCID 27364482-Ethyl-6-methylphenyl isocyanateHCID 178506595HCID 178506595、化合物

生成物 1

HCID 178436207HCID 178436207、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

In a manner similar to that previously described, 15.55 grams (0.073 mole) of 2-iminoimidazoline hydroiodide is added dropwise to a dry cooled suspension of 596 milligrams (0.075 mole) of lithium hydride in 30 milliliters of dimethylformamide under an atmosphere of nitrogen. After completion of the addition, the mixture is allowed to warm to room temperature to complete the reaction. Thereafter the mixture is again cooled, a solution of 8.1 grams (0.05 mole) of 2-ethyl-6-methylphenyl isocyanate in 25 milliliters of dry dimethylformamide is added dropwise over a two hour period and then after the resulting mixture is stirred overnight while the temperature is allowed to rise to ambient temperatures to obtain a N-(2-ethyl-6-methylphenyl)-N'-(2-imidazolidinylidene)urea product. The base product is recovered by procedures similar to that previously described and after recrystallization from methanol-water, a purified base product, m.p. 185°-187° C. is obtained.

後処理

  1. temperaturecooled
  2. additionAfter completion of the addition
  3. customthe reaction
  4. temperatureThereafter the mixture is again cooled

出典と根拠

ORDレコード
ord-45bdcf1f11ec4d2dbe6b1e5eef3946bd
出典データセット
uspto-grants-1980_10
特許番号
US04229462

反応ノート

読み込み中…