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Hydrochloric Acid → HCID 86585628, 화합물

HRID 50441
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HRID 50441 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12](=[O:44])[O:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([NH:22][C:23]3[CH:28]=[C:27]([Cl:29])[C:26]([C:30]([F:33])([F:32])[F:31])=[CH:25][C:24]=3[NH:34][C:35]([C:37]3[CH:41]=[C:40]([CH3:42])[N:39]([CH3:43])[N:38]=3)=O)=[CH:18][CH:17]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1.Cl>[OH-].[Na+].C(O)C.O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([NH:11][C:12](=[O:44])[O:13][CH2:14][CH2:15][C:16]2[CH:21]=[CH:20][C:19]([N:22]3[C:23]4[CH:28]=[C:27]([Cl:29])[C:26]([C:30]([F:32])([F:31])[F:33])=[CH:25][C:24]=4[N:34]=[C:35]3[C:37]3[CH:41]=[C:40]([CH3:42])[N:39]([CH3:43])[N:38]=3)=[CH:18][CH:17]=2)(=[O:10])=[O:9])=[CH:4][CH:3]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 2

HCID 313Hydrochloric AcidHCID 865856292-(4-{[5-chloro-2-{[(1,5-dimethyl-1H-pyrazol-3-yl)carbonyl]amino}-4-(trifluoromethyl)phenyl]amino}phenyl)ethyl (4-methylphenyl)sulfonylcarbamate

생성물 1

HCID 86585628HCID 86585628, 화합물수율 21.3%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매
HCID 14798
Sodium Hydroxide
용매

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온도
50 °C

실험 절차

A mixture of 2-(4-{[5-chloro-2-{[(1,5-dimethyl-1H-pyrazol-3-yl)carbonyl]amino}-4-(trifluoromethyl)phenyl]amino}phenyl)ethyl (4-methylphenyl)sulfonylcarbamate (step 3, 145 mg, 0.223 mmol) in 2N NaOH (1 ml) and ethanol (2 ml) was stirred at 50° C. for 85 h. After cooling, the pH value was adjusted to 4.0 by addition of 2N HCl. The mixture was diluted with water (80 ml), and extracted with dichloromethane (80 ml×3). The combined organic layer was washed with brine (50 ml), dried (MgSO4), and concentrated. Purification by PTLC eluting with hexane/ethyl acetate (1:3) to afford 30 mg (21%) of the title compound as a red solid.

후처리

  1. temperatureAfter cooling
  2. extractionextracted with dichloromethane (80 ml×3)
  3. washThe combined organic layer was washed with brine (50 ml)
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated
  6. customPurification by PTLC
  7. washeluting with hexane/ethyl acetate (1:3)

출처 및 근거

ORD 기록
ord-8d8a474b3a1c46dc911ff809570e3a0a
출처 데이터셋
uspto-grants-2004_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06710054B2

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