Hydrochloric Acid → 4-{5-[1-(4-Methyl-piperazin-1-ylmethyl)-cyclopropyl]-4-phenyl-isoxazol-3-yl}-phenol

HRID 2378052노트

반응식

HRID 2378052 반응식
COC[O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[C:15]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)=[C:14]([C:22]3([CH2:25][N:26]4[CH2:31][CH2:30][N:29]([CH3:32])[CH2:28][CH2:27]4)[CH2:24][CH2:23]3)[O:13][N:12]=2)=[CH:7][CH:6]=1.Cl.[OH-].[Na+]>C(O)(C)C>[CH3:32][N:29]1[CH2:28][CH2:27][N:26]([CH2:25][C:22]2([C:14]3[O:13][N:12]=[C:11]([C:8]4[CH:9]=[CH:10][C:5]([OH:4])=[CH:6][CH:7]=4)[C:15]=3[C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=3)[CH2:23][CH2:24]2)[CH2:31][CH2:30]1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 689564541-{1-[3-(4-Methoxymethoxy-phenyl)-4-phenyl-isoxazol-5-yl]-cyclopropylmethyl}-4-methyl-piperazine

생성물 1

HCID 1363896464-{5-[1-(4-Methyl-piperazin-1-ylmethyl)-cyclopropyl]-4-phenyl-isoxazol-3-yl}-phenol

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

To a mixture consisting of 1-{1-[3-(4-methoxymethoxy-phenyl)-4-phenyl-isoxazol-5-yl]-cyclopropylmethyl}-4-methyl-piperazine (this example, Step B) in isopropanol is added 6 N hydrochloric acid solution. The mixture is stirred at room temperature overnight. The mixture is titrated to pH 8 with an aqueous sodium hydroxide solution and is extracted with ethyl acetate. The organic layer is separated and dried over anhydrous sodium sulfate. The mixture is filtered and the filtrate is concentrated under reduced pressure. The concentrate is purified to afford the title compound 1H NMR (400 MHz, CDCl3) δ 7.40-7.20 (m, 7H), 6.70 (d, 2H), 2.45 (m, 8H), 2.25 (s, 3H), 1.05 (m, 2H), 0.78 (m, 2H); MS (EH+) m/z 390 (MH+.)

후처리

  1. extractionis extracted with ethyl acetate
  2. customThe organic layer is separated
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationThe mixture is filtered
  5. concentrationthe filtrate is concentrated under reduced pressure
  6. customThe concentrate is purified

출처 및 근거

ORD 기록
ord-0a4448c9c1834f059b66be5e6d967d78
출처 데이터셋
uspto-grants-2008_12
특허 번호
US07470715B2

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