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Methyl 5-methoxy-3-oxopentanoate → HCID 178494792, 화합물

HRID 636431
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HRID 636431 반응식
[C:1]1([S:7]([C:10]2[C:14]([S:15][CH3:16])=[N:13][NH:12][C:11]=2[NH2:17])(=[O:9])=[O:8])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C[O:19][CH2:20][CH2:21][C:22](=O)[CH2:23][C:24]([O:26][CH3:27])=O>C(O)(=O)C>[C:1]1([S:7]([C:10]2[C:14]([S:15][CH3:16])=[N:13][N:12]3[C:20]([OH:19])=[CH:21][C:22]([CH2:23][CH2:24][O:26][CH3:27])=[N:17][C:11]=23)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 542416Methyl 5-methoxy-3-oxopentanoateHCID 110547174-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine

생성물 1

HCID 178494792HCID 178494792, 화합물수율 61%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2.69 g (10 mmol) of) 4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine and 1.6 g (10 mmol) of methyl 5-methoxy-3-oxo-valerate in 10 ml of acetic acid was heated at reflux for 4 hrs. The reaction solution was evaporated and the residue was partitioned between H2O and CH2Cl2. The aqueous phase was extracted three times with 80 ml of CH2Cl2. The combined organic phases were dried (MgSO4), filtered and evaporated. Chromatography (SiO2, CH2Cl2/MeOH 20:1) yielded 2.40 g (61%) of 3-benzenesulphonyl-5-(2-methoxy-ethyl)-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ol as a beige powder.

후처리

  1. temperatureat reflux for 4 hrs
  2. customThe reaction solution was evaporated
  3. customthe residue was partitioned between H2O and CH2Cl2
  4. extractionThe aqueous phase was extracted three times with 80 ml of CH2Cl2
  5. dry with materialThe combined organic phases were dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated

출처 및 근거

ORD 기록
ord-a7f256e765f74f1fb1433246f2979beb
출처 데이터셋
uspto-grants-2001_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06194410B1

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