Hydrochloric Acid → 2-(3-ethoxy-3-oxopropyl)-4-{[1-isopentyl-4-(3-methylbutanoyl)-1H-pyrrol-2-yl]carbonyl}phenyl 3-methylbutanoate

HRID 2249654

반응식

HRID 2249654 반응식
[CH3:1][CH:2]([CH3:33])[CH2:3][C:4]([O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([C:15]2[NH:16][CH:17]=[C:18]([C:20](=[O:25])[CH2:21][CH:22]([CH3:24])[CH3:23])[CH:19]=2)=[O:14])=[CH:9][C:8]=1[CH2:26][CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:5].[H-].[Na+].[CH2:36](I)[CH2:37][CH:38]([CH3:40])[CH3:39].Cl>CN(C)C=O.O.C(OCC)(=O)C>[CH3:1][CH:2]([CH3:33])[CH2:3][C:4]([O:6][C:7]1[CH:12]=[CH:11][C:10]([C:13]([C:15]2[N:16]([CH2:36][CH2:37][CH:38]([CH3:40])[CH3:39])[CH:17]=[C:18]([C:20](=[O:25])[CH2:21][CH:22]([CH3:23])[CH3:24])[CH:19]=2)=[O:14])=[CH:9][C:8]=1[CH2:26][CH2:27][C:28]([O:30][CH2:31][CH3:32])=[O:29])=[O:5]

참가 물질

8

반응물 4

HCID 313Hydrochloric AcidHCID 109241-Iodo-3-methylbutaneHCID 24758Sodium hydrideHCID 178165282-(3-ethoxy-3-oxopropyl)-4-{[4-(3-methylbutanoyl)-1H-pyrrol-2-yl]carbonyl}phenyl 3-methylbutanoate

생성물 1

HCID 178164722-(3-ethoxy-3-oxopropyl)-4-{[1-isopentyl-4-(3-methylbutanoyl)-1H-pyrrol-2-yl]carbonyl}phenyl 3-methylbutanoate

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
55 °C

실험 절차

To a solution of 0.9 g of 2-(3-ethoxy-3-oxopropyl)-4-{[4-(3-methylbutanoyl)-1H-pyrrol-2-yl]carbonyl}phenyl 3-methylbutanoate in 18 ml N,N-dimethylformamide are added 0.12 g of 60% sodium hydride and 0.4 ml of isopentyl iodide successively, and the mixture thus obtained is stirred at 50-60° C. for one hour. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 6 mol/L hydrochloric acid, and the organic layer is separated. The organic layer is washed with water and saturated aqueous solution of sodium chloride and dried over anhydrous magnesium sulfate, and the solvent is distilled off under reduced pressure. Thus, 0.7 g of 2-(3-ethoxy-3-oxopropyl)-4-{[1-isopentyl-4-(3-methylbutanoyl)-1H-pyrrol-2-yl]carbonyl}phenyl 3-methylbutanoate is obtained as a white solid product.

후처리

  1. customthe mixture thus obtained
  2. customthe organic layer is separated
  3. washThe organic layer is washed with water and saturated aqueous solution of sodium chloride
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-e2824c757c6443cc8fe4518d95ad7541
출처 데이터셋
uspto-grants-2008_01
특허 번호
US07314888B1

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