Lithium hydride → HCID 178436207、化合物

HRID 1732887ノート

反応式

HRID 1732887 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 thereafter 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-727d590dbda04da38ccc9636e9ab8e2a
出典データセット
uspto-grants-1980_12
特許番号
US04239768

反応ノート

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