4-Chloroaniline → N-(4-Chlorophenyl)-N'-(1-methoxy-2-methyl-1-oxopropan-2-yl)carbamimidic acid

HRID 224943

반응식

HRID 224943 반응식
[CH3:1][O:2][C:3](=[O:10])[C:4]([N:7]=[C:8]=[O:9])([CH3:6])[CH3:5].[Cl:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1>O1CCCC1>[CH3:1][O:2][C:3](=[O:10])[C:4]([CH3:6])([CH3:5])[NH:7][C:8](=[O:9])[NH:16][C:15]1[CH:17]=[CH:18][C:12]([Cl:11])=[CH:13][CH:14]=1

참가 물질

4

반응물 2

HCID 78124-ChloroanilineHCID 2769374Methyl 2-isocyanato-2-methylpropanoate

생성물 1

HCID 1252008N-(4-Chlorophenyl)-N'-(1-methoxy-2-methyl-1-oxopropan-2-yl)carbamimidic acid

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of 17.0 g (119 mmol) of 2-isocyanato-2-methylpropionic acid methyl ester in 150 ml of absolute tetrahydrofuran was added, over a 15 minute period to 15.1 g (119 mmol) of p-chloroaniline in 300 ml of absolute tetrahydrofuran. After refluxing the mixture for three days, the solution was evaporated to dryness. The product, after two recrystallizations from methylene chloride, was dried for 6 hours at 40° C., under greatly reduced pressure, to yield N-[(4-chlorophenyl)-carbamoyl]-2-methylalanine methyl ester, m.p. 147°-148° C.

후처리

  1. temperatureAfter refluxing the mixture for three days
  2. customthe solution was evaporated to dryness
  3. customThe product, after two recrystallizations from methylene chloride
  4. customwas dried for 6 hours at 40° C., under greatly reduced pressure

출처 및 근거

ORD 기록
ord-4cf93b30dd0545c882f2b28327abb08d
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234736

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