1-(2-Methoxyphenyl)piperazine → 3-[4-(2-Methoxyphenyl)piperazinyl]-2-phenylpropionic acid

HRID 37364

반응식

HRID 37364 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.[C:15]([OH:25])(=[O:24])[C:16]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)=[CH2:17]>C(O)C>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]1[CH2:14][CH2:13][N:12]([CH2:17][CH:16]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[C:15]([OH:25])=[O:24])[CH2:11][CH2:10]1

참가 물질

4

반응물 2

HCID 13461-(2-Methoxyphenyl)piperazineHCID 68114Atropic acid

생성물 1

HCID 100886143-[4-(2-Methoxyphenyl)piperazinyl]-2-phenylpropionic acid

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

1-(2-Methoxyphenyl)piperazine (22.6 g; 0.118 mol) and atropic acid (174 g, 0.118 moll in ethanol (300 ml) were heated under reflux for 18 hours, cooled to room temperature, and evaporated in vacuo. The solid was triturated with acetone (3×100 ml) to give a first crop of product (13.8 g) as white crystals. The filtrate was evaporated in vacuo to give an oil which slowly crystallised over 1 month. The solid was triturated with acetone (200 ml) to give a second crop of the hemihydrate of the product (9.01 g) as white crystals, m.p. 160°-163°. (Found: C, 68.4; H, 7.2; N, 7.9. C20H24N2O3.0.5H2O requires C, 68.8; H, 7.2; N, 8.0%.)

후처리

  1. temperatureunder reflux for 18 hours
  2. customevaporated in vacuo
  3. customThe solid was triturated with acetone (3×100 ml)

출처 및 근거

ORD 기록
ord-ccae9be3c5eb46ebbf97353a9823ff7c
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420278

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