Pyridine → N-(2,6-diisopropylphenyl)-N'-(4-tert-butylcyclohexyl)urea

HRID 37291

반응식

HRID 37291 반응식
[C:1]([CH:5]1[CH2:10][CH2:9][CH:8]([NH2:11])[CH2:7][CH2:6]1)([CH3:4])([CH3:3])[CH3:2].[CH:12]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH:21]([CH3:23])[CH3:22])[C:16]=1[N:24]=[C:25]=[O:26])([CH3:14])[CH3:13].N1C=CC=CC=1>ClCCl>[CH:12]([C:15]1[CH:20]=[CH:19][CH:18]=[C:17]([CH:21]([CH3:22])[CH3:23])[C:16]=1[NH:24][C:25]([NH:11][CH:8]1[CH2:7][CH2:6][CH:5]([C:1]([CH3:4])([CH3:2])[CH3:3])[CH2:10][CH2:9]1)=[O:26])([CH3:13])[CH3:14]

참가 물질

5

반응물 3

HCID 1049PyridineHCID 793964-tert-ButylcyclohexylamineHCID 922592,6-Diisopropylphenyl isocyanate

생성물 1

HCID 19935041N-(2,6-diisopropylphenyl)-N'-(4-tert-butylcyclohexyl)urea수율 59.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To a solution of 1.6 g of 4-tert-butylcyclohexylamine in 15 ml of dichloromethane was added a solution of 2.2 g of 2,6-diisopropylphenylisocyanate in dichloromethane dropwise in the presence of pyridine at 0° C. Thereafter the mixture was stirred for 1.5 hours at room temperature and concentrated. The residue was partitioned between isopropyl ether and water, and the organic layer was successively washed with 0.5N hydrochloric acid, water and sodium sulfate solution. The organic layer was dried over magnesium sulfate and then distilled away. The resulting residue was crystallized from ethyl acetate to give 2.2 g of N-(2,6-diisopropylphenyl)-N'-(4-tert-butylcyclohexyl)urea, melting at 270° C.

후처리

  1. concentrationconcentrated
  2. customThe residue was partitioned between isopropyl ether and water
  3. washthe organic layer was successively washed with 0.5N hydrochloric acid, water and sodium sulfate solution
  4. dry with materialThe organic layer was dried over magnesium sulfate
  5. distillationdistilled away
  6. customThe resulting residue was crystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-6a6b231c3e824992b74412a4122da314
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420164

연결된 노트

불러오는 중…