Toluene → Cyclopentylurea

HRID 1580462

反応式

HRID 1580462 の反応式
[NH2:1][C:2]([NH2:4])=[O:3].[C:5]1([CH3:11])[CH:10]=[CH:9][CH:8]=CC=1.CCOCC.C1(N)CCCC1>C(O)(=O)C>[CH:8]1([NH:1][C:2](=[O:3])[NH2:4])[CH2:9][CH2:10][CH2:5][CH2:11]1

参加物

6

反応物 4

HCID 1140TolueneHCID 1176UreaHCID 2906CyclopentylamineHCID 3283Diethyl Ether

生成物 1

HCID 294526Cyclopentylurea

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of 10.3 g of N-[4-(β-<2-methoxy-5-chlorobenzamido>-ethyl)-benzenesulfonyl]-urea (m.p. 171° - 173°C), 300 ml of toluene, 30 ml of glycolmonomethyl ether, 1.65 g of glacial acetic acid and 2.4 g of cyclopentyl-amine was refluxed for 5 hours. Subsequently, the mixture was concentrated in vacuo and the residue was treated with alcohol. N-[4-(β-<2-methoxy-5-chlorobenzamido>-ethyl)-benzenesulfonyl] -N'-cyclopentyl-urea obtained as a raw product was separated by suction-filtration and recrystallized from methanol. Melting point 184° - 185°C.

後処理

  1. temperaturewas refluxed for 5 hours
  2. concentrationSubsequently, the mixture was concentrated in vacuo
  3. additionthe residue was treated with alcohol

出典と根拠

ORDレコード
ord-ea12b79f021d43b8bfd49fcd431891af
出典データセット
uspto-grants-1976_01
特許番号
US03932658

関連ノート

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