Urea → Ethyl N-(aminocarbonyl)carbamate

HRID 1164467

반응식

HRID 1164467 반응식
[C:1]([O:6]C([O-])=O)(=O)[O:2][CH2:3][CH3:4].[NH2:10][C:11]([NH2:13])=[O:12]>C(Cl)(Cl)Cl>[C:1]([NH:10][C:11](=[O:12])[NH2:13])([O:2][CH2:3][CH3:4])=[O:6]

참가 물질

4

반응물 2

HCID 1176UreaHCID 86738757HCID 86738757, 화합물

생성물 1

HCID 69380Ethyl N-(aminocarbonyl)carbamate

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

0.65 ml (0.72 g, 0.00443 moles) of ethyl pyrocarbonate are added to a solution of 1.0 g (0.00285 moles) of 1-(1',3'-bis/2",6"-dimethylphenyl/-4'-methyl-imidazolidine-2'-ylidene)-urea, prepared as described in Example 72, in 10 ml of dry chloroform, and the mixture is allowed to stand at room temperature for 48 hours. Thereafter the solvent and the excess of the reactant are distilled off under reduced pressure. The oily residue is dissolved in 10 ml of diethyl ether, the insolubles are filtered off, and the filtrate is concentrated to a final volume of about 2 ml. Next day the separated crystalline product is filtered off, washed with a small amount of diethyl ether and dried. 0.5 g (41.7%) of 1-(1',3'-bis/2",6"-dimethylphenyl/-4'-methyl-imidazolidine-2'-ylidene)-3-carbethoxy-urea are obtained; m.p.: 123°-125° C.

후처리

  1. customprepared
  2. distillationThereafter the solvent and the excess of the reactant are distilled off under reduced pressure
  3. dissolutionThe oily residue is dissolved in 10 ml of diethyl ether
  4. filtrationthe insolubles are filtered off
  5. concentrationthe filtrate is concentrated to a final volume of about 2 ml
  6. filtrationNext day the separated crystalline product is filtered off
  7. washwashed with a small amount of diethyl ether
  8. customdried

출처 및 근거

ORD 기록
ord-7a34ac528a9d4747be3a1a2afc67091f
출처 데이터셋
uspto-grants-1983_01
특허 번호
US04369325

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