Lithium hydride → HCID 178436207, 화합물

HRID 903906노트

반응식

HRID 903906 반응식
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]

참가 물질

5

반응물 3

HCID 62714Lithium hydrideHCID 27364482-Ethyl-6-methylphenyl isocyanateHCID 178506595HCID 178506595, 화합물

생성물 1

HCID 178436207HCID 178436207, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-45bdcf1f11ec4d2dbe6b1e5eef3946bd
출처 데이터셋
uspto-grants-1980_10
특허 번호
US04229462

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