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Acetic Acid → HCID 21940006, 화합물

HRID 1242941
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HRID 1242941 반응식
S(=O)(=O)(O)O.[C:6]([OH:9])(=[O:8])[CH3:7].[Cl:10][C:11]1[CH:16]=[CH:15][C:14]([C:17]2[CH:22]=[CH:21][C:20]([C:23]([NH:25][C:26]3[CH:31]=[CH:30][C:29]([CH:32](O)[CH:33]4[CH2:38][CH2:37][CH2:36][N:35](C(OC(C)(C)C)=O)[CH2:34]4)=[CH:28][CH:27]=3)=[O:24])=[CH:19][CH:18]=2)=[CH:13][CH:12]=1>C(OCC)(=O)C>[C:6]([O:9][CH:32]([C:29]1[CH:28]=[CH:27][C:26]([NH:25][C:23]([C:20]2[CH:21]=[CH:22][C:17]([C:14]3[CH:13]=[CH:12][C:11]([Cl:10])=[CH:16][CH:15]=3)=[CH:18][CH:19]=2)=[O:24])=[CH:31][CH:30]=1)[CH:33]1[CH2:38][CH2:37][CH2:36][NH:35][CH2:34]1)(=[O:8])[CH3:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 1118Sulfuric AcidHCID 21939926HCID 21939926, 화합물

생성물 1

HCID 21940006HCID 21940006, 화합물

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Concentrated sulfuric acid (0.0562 ml) was added to an acetic acid solution (3.5 ml) of tert-butyl 3-[[4-[[(4′-chloro[1,1′-biphenyl]-4-yl)carbonyl]amino]phenyl](hydroxy)methyl]-1-piperidinecarboxylate (366 mg, 0.702 mmol) obtained in Example 128, which was stirred under room temperature for 16 hours. Ethyl acetate was added to the reaction mixture, which was washed with potassium hydrogencarbonate solution and saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate, and then the solvent was distilled out under reduced pressure. The resulting oily substance was purified by alumina B column chromatography (development solvent; ethyl acetate: methanol=3:1), and powdered with diisopropyl ether, to give the titled compound (210 mg).

후처리

  1. washwas washed with potassium hydrogencarbonate solution and saturated aqueous sodium chloride solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. distillationthe solvent was distilled out under reduced pressure
  4. customThe resulting oily substance was purified by alumina B column chromatography (development solvent; ethyl acetate: methanol=3:1)

출처 및 근거

ORD 기록
ord-4b34b234d33b4d4db197bb8b74f5d116
출처 데이터셋
uspto-grants-2006_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07115750B1

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