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Hydrochloric Acid → 2-Acetyl-5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone hydrochloride

HRID 1612949
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HRID 1612949 반응식
[CH:1]1([O:6][C:7]2[CH:8]=[C:9]([CH:15]3[N:19]([CH3:20])[NH:18][C:17](=[O:21])[CH2:16]3)[CH:10]=[CH:11][C:12]=2[O:13][CH3:14])[CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:22].[C:23](OC(=O)C)(=[O:25])[CH3:24]>CCOCC>[ClH:22].[C:23]([N:18]1[C:17](=[O:21])[CH2:16][CH:15]([C:9]2[CH:10]=[CH:11][C:12]([O:13][CH3:14])=[C:7]([O:6][CH:1]3[CH2:2][CH2:3][CH2:4][CH2:5]3)[CH:8]=2)[N:19]1[CH3:20])(=[O:25])[CH3:24]
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 7918Acetic AnhydrideHCID 197927655-[3-(Cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone

생성물 1

HCID 197927892-Acetyl-5-[3-(cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone hydrochloride수율 98%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

5-[3-(Cyclopentyloxy)-4-methoxyphenyl]-1-methyl-3-pyrazolidinone (0.500 g) is dissolved in acetic anhydride (15 mL). The resulting solution is warmed to reflux for 2 hours, cooled to room temperature and concentrated in vacuo to afford an oil. This residue is dissolved in ether and treated with ethanolic HCl at room temperature. The resulting solid is stirred for 4 hours at room temperature, collected by suction and dried in vacuo to afford the title compound as a white powder (0.621 g; 98%) mp: 82°-85° C. 1H NMR (DMSO-d6, 400 MHz) δ6.88 (m, 3H); 3.85 (s, 3H); 2.82 (s, 3H); 2.52 (s, 3H); 2.00 (m, 2H); 1.84 (m, 3H); 1.64 (m, 2H). IR (KBr, cm-1) 1730.

후처리

  1. temperatureThe resulting solution is warmed
  2. temperatureto reflux for 2 hours
  3. concentrationconcentrated in vacuo
  4. customto afford an oil
  5. customcollected by suction
  6. customdried in vacuo

출처 및 근거

ORD 기록
ord-ab47c019473347648edb80b5d9b6419b
출처 데이터셋
uspto-grants-1993_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05191084

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