(E)-3-[2-[4-(cyclobutyl)-2-thiazolyl]ethenyl]benzeneamine → (E)-2-[3-[3-[2-[4-(cyclobutyl)-2-thiazolyl]ethenyl]phenylamino]-3-oxopropyl]benzoic acid ethyl ester

HRID 327574ノート

反応式

HRID 327574 の反応式
[CH2:1]([O:3][C:4]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][CH2:13][C:14]([OH:16])=O)=[O:5])[CH3:2].[CH:17]1([C:21]2[N:22]=[C:23](/[CH:26]=[CH:27]/[C:28]3[CH:29]=[C:30]([NH2:34])[CH:31]=[CH:32][CH:33]=3)[S:24][CH:25]=2)[CH2:20][CH2:19][CH2:18]1>CN(C)C1C=CN=CC=1.C(Cl)Cl>[CH2:1]([O:3][C:4](=[O:5])[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][C:7]=1[CH2:12][CH2:13][C:14]([NH:34][C:30]1[CH:31]=[CH:32][CH:33]=[C:28](/[CH:27]=[CH:26]/[C:23]2[S:24][CH:25]=[C:21]([CH:17]3[CH2:20][CH2:19][CH2:18]3)[N:22]=2)[CH:29]=1)=[O:16])[CH3:2]

参加物

5

実験手順

A solution composed of 0.44 g of 2-(ethoxycarbonyl)benzenepropanoic acid and 25 ml of methylene chloride was added to a solution composed of 0.51 g of (E)-3-[2-[4-(cyclobutyl)-2-thiazolyl]ethenyl]benzeneamine, 0.4 g of N-ethyl-N-(dimethylaminopropyl)carbodiimide, 1.0 g of 4-dimethylaminopyridine and 25 ml of methylene chloride at 0° C. After 16 hr., the reaction mixture was washed with 30 ml of water, dried (MgSO4) and the solvents removed by rotary evaporation. The residual materials were recrystallized from ethyl ether to yield 0.87 g of (E)-2-[3-[3-[2-[4-(cyclobutyl)-2-thiazolyl]ethenyl]phenylamino]-3-oxopropyl]benzoic acid ethyl ester; m.p.110°-111° C.

後処理

  1. additionwas added to a solution
  2. wash, the reaction mixture was washed with 30 ml of water
  3. dry with materialdried (MgSO4)
  4. customthe solvents removed by rotary evaporation
  5. customThe residual materials were recrystallized from ethyl ether

出典と根拠

ORDレコード
ord-8ad9756cebe540d6a69be0934337860b
出典データセット
uspto-grants-1993_12
特許番号
US05273986

反応ノート

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