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

HRID 37291

反応式

HRID 37291 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6a6b231c3e824992b74412a4122da314
出典データセット
uspto-grants-1995_05
特許番号
US05420164

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