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Hydrochloric Acid → HCID 56941127, 화합물

HRID 1844027
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HRID 1844027 반응식
Cl.C([N:5]1[C:17]2[CH:16]=[C:15]3[C:10]([CH2:11][CH2:12][N:13]([C:19]4[CH:20]=[N:21][CH:22]=[CH:23][C:24]=4[CH3:25])[C:14]3=[O:18])=[CH:9][C:8]=2[CH:7]=[N:6]1)(=O)C.C(OCC)(=O)C>CO>[CH3:25][C:24]1[CH:23]=[CH:22][N:21]=[CH:20][C:19]=1[N:13]1[CH2:12][CH2:11][C:10]2[C:15](=[CH:16][C:17]3[NH:5][N:6]=[CH:7][C:8]=3[CH:9]=2)[C:14]1=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 89964093HCID 89964093, 화합물

생성물 1

HCID 56941127HCID 56941127, 화합물수율 11.5%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

6N HCl (5 mL) was added drop wise to a solution of 1-acetyl-7-(4-methylpyridin-3-yl)-6,7-dihydro-1H-pyrazolo[4,3-g]isoquinolin-8(5H)-one (I-69h: 80 mg, 0.249 mmol) in methanol (5 ml) at 0° C. and the resulting reaction mass was stirred at room temperature for 36 hours. The reaction was monitored by TLC (100% ethyl acetate). The reaction mass was concentrated under reduced pressure, basified using saturated NaHCO3 solution and extracted using ethyl acetate. The organic layer was dried over Na2SO4 and concentrated under reduced pressure to afford the crude product. Purification by column chromatography on silica gel (100% ethyl acetate), followed by preparative HPLC afforded 8 mg of the product (11.5% yield).

후처리

  1. customthe resulting reaction mass
  2. concentrationThe reaction mass was concentrated under reduced pressure
  3. extractionextracted
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customto afford the crude product
  7. customPurification by column chromatography on silica gel (100% ethyl acetate)

출처 및 근거

ORD 기록
ord-b27796adb9b7425fa7b7c50ec805e11f
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08946260B2

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