Water → Ethyl[1-(4-aminosulfonylphenyl)-5-(4-chlorophenyl)-1H-pyrazole-3-yl]carboxylate

HRID 1292306노트

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HRID 1292306 반응식
[CH3:1][O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)[N:7]([C:17]2[CH:22]=[CH:21][C:20]([S:23]([NH2:26])(=[O:25])=[O:24])=[CH:19][CH:18]=2)[N:6]=1)=[O:4].[CH3:27]C[O-].[Na+].CCO.O>C(O)C>[CH2:1]([O:2][C:3]([C:5]1[CH:9]=[C:8]([C:10]2[CH:15]=[CH:14][C:13]([Cl:16])=[CH:12][CH:11]=2)[N:7]([C:17]2[CH:22]=[CH:21][C:20]([S:23]([NH2:26])(=[O:25])=[O:24])=[CH:19][CH:18]=2)[N:6]=1)=[O:4])[CH3:27]

참가 물질

5

반응물 3

HCID 962WaterHCID 3289819methyl 1-[4-(aminosulfonyl)phenyl]-5-(4-chlorophenyl)-1H-pyrazole-3-carboxylateHCID 23706232Ethanol sodium ethoxide

생성물 1

HCID 9844224Ethyl[1-(4-aminosulfonylphenyl)-5-(4-chlorophenyl)-1H-pyrazole-3-yl]carboxylate수율 70%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
0 °C

실험 절차

Methyl[1-(4-aminosulfonylphenyl)-5-(4-chlorophenyl)-1H-pyrazole-3-yl]carboxylate (Example 85) (0.10 g) was dissolved in absolute ethanol (10 mL) and a catalytic amount of 21% NaOEt/EtOH was added. The reaction was stirred without temperature control for 72 hours, then water (10 mL) was added. The product crystallized, the suspension was cooled to 0° C. and held for 30 minutes. The product was filtered, washed with water (5 mL) and dried to yield 0.071 g (70%) of a white solid: Mass Spectrum: MH+=406. Anal. Calc'd for C18H16N3O4ClS: C, 53.27; H, 3.97; N, 10.35; Cl, 8.74; S, 7.90. Found: C, 53.04; H, 4.00; N, 10.27; Cl, 8.69; S, 7.97.

후처리

  1. customThe product crystallized
  2. waitheld for 30 minutes
  3. filtrationThe product was filtered
  4. washwashed with water (5 mL)
  5. customdried

출처 및 근거

ORD 기록
ord-130ad2ed0e28488c85110c6205c1cb0f
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05756529

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