1-Piperazinecarboxylic acid, ethyl ester → HCID 14987925, 화합물

HRID 1494267노트

반응식

HRID 1494267 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 14987925HCID 14987925, 화합물수율 80.1%

시약·촉매·용매 1

HCID 7237O-Xylene용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-c752dc77e3b44a7d98a3abd86b775d1c
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05025012

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