1-Piperazinecarboxylic acid, ethyl ester → HCID 14987925、化合物

HRID 1494267ノート

反応式

HRID 1494267 の反応式
[N:1]1([C:7]([O:9][CH2:10][CH3:11])=[O:8])[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:13]1[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][N:14]=1>C1(C)C(C)=CC=CC=1>[CH2:10]([O:9][C:7]([N:1]1[CH2:6][CH2:5][N:4]([C:13]2[CH:21]=[CH:20][C:16]([C:17]([OH:19])=[O:18])=[CH:15][N:14]=2)[CH2:3][CH2:2]1)=[O:8])[CH3:11]

参加物

4

反応物 2

HCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 792226-Chloronicotinic acid

生成物 1

HCID 14987925HCID 14987925、化合物収率 80.1%

試薬・触媒・溶媒 1

HCID 7237O-Xylene溶媒

実験手順

A mixture of 10.1 g of ethyl 1-piperazine carboxylate, 5.0 g of 6-chloronicotinic acid and 15 ml of xylene was stirred at 140°-150° C. for 3 hours. After cooled crystals were filtered, to the crystals was added a solution of 2.6 g of sodium hydroxide in 30 ml of water followed by extraction with toluene. Concentrated hydrochloric acid was added to the aqueous layer, and crystals precipitated were filtered, washed with water and dried to afford 7.1 g of 6-(4-ethoxycarbonyl-1-piperazinyl)nicotinic acid (yield 80%).

後処理

  1. temperatureAfter cooled crystals
  2. filtrationwere filtered, to the crystals
  3. additionwas added a solution of 2.6 g of sodium hydroxide in 30 ml of water
  4. extractionfollowed by extraction with toluene
  5. additionConcentrated hydrochloric acid was added to the aqueous layer, and crystals
  6. customprecipitated
  7. filtrationwere filtered
  8. washwashed with water
  9. customdried

出典と根拠

ORDレコード
ord-c752dc77e3b44a7d98a3abd86b775d1c
出典データセット
uspto-grants-1991_06
特許番号
US05025012

反応ノート

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