4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine → HCID 178494547, 화합물

HRID 636434

반응식

HRID 636434 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][C:21](=O)[CH2:22][C:23]([O:25][CH2:26]C)=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][O:25][CH3:26])=[N:17][C:11]=23)(=[O:9])=[O:8])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 110547174-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamineHCID 12645099Ethyl 4-methoxy-3-oxobutanoate

생성물 1

HCID 178494547HCID 178494547, 화합물수율 85%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

A solution of 2.69 g (10 mmol) 4-benzenesulphonyl-5-methylsulphanyl-2H-pyrazol-3-ylamine and 1.46 g (10 mmol) of ethyl 4-methoxy-acetoacetate in 10 ml of acetic acid was heated at reflux for 3 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 25:1) yielded 3.1 g (85%) of 3-benzenesulphonyl-5-methoxymethyl-2-methylsulphanyl-pyrazolo[1,5-a]pyrimidin-7-ol as a beige powder, m.p. 175-155°.

후처리

  1. temperatureat reflux for 3 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-71c13a4487e84535bdbd8749a6661bb8
출처 데이터셋
uspto-grants-2001_02
특허 번호
US06194410B1

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