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N-(1-(1-(4-chlorophenyl)-1-(2-cyanocyclopropyl)propyl)-1H-indazol-4-yl)-N-((2-(trimethylsilyl)ethoxy)methyl)methanesulfonamide → N-(1-(1-(4-chlorophenyl)-1-(2-cyanocyclopropyl)propyl)-1H-indazol-4-yl)methanesulfonamide

HRID 1477865
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HRID 1477865 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:16]2[C:24]3[C:19](=[C:20]([N:25](COCC[Si](C)(C)C)[S:26]([CH3:29])(=[O:28])=[O:27])[CH:21]=[CH:22][CH:23]=3)[CH:18]=[N:17]2)([CH:11]2[CH2:13][CH:12]2[C:14]#[N:15])[CH2:9][CH3:10])=[CH:4][CH:3]=1>Cl.CCO>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]([N:16]2[C:24]3[C:19](=[C:20]([NH:25][S:26]([CH3:29])(=[O:28])=[O:27])[CH:21]=[CH:22][CH:23]=3)[CH:18]=[N:17]2)([CH:11]2[CH2:13][CH:12]2[C:14]#[N:15])[CH2:9][CH3:10])=[CH:4][CH:3]=1
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참가 물질

3

반응물 1

HCID 70563960N-(1-(1-(4-chlorophenyl)-1-(2-cyanocyclopropyl)propyl)-1H-indazol-4-yl)-N-((2-(trimethylsilyl)ethoxy)methyl)methanesulfonamide

생성물 1

HCID 57524237N-(1-(1-(4-chlorophenyl)-1-(2-cyanocyclopropyl)propyl)-1H-indazol-4-yl)methanesulfonamide

시약·촉매·용매 1

HCID 21887872Ethanol hydrochloride용매

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온도
50 °C

실험 절차

A mixture of N-(1-(1-(4-chlorophenyl)-1-(2-cyanocyclopropyl)propyl)-1H-indazol-4-yl)-N-((2-(trimethylsilyl)ethoxy)methyl)methanesulfonamide (14 mg) in 2 N HCl/EtOH (1 mL/1 mL) was stirred at 50° C. for 3 h, cooled to room temperature, concentrated, and extracted with ethyl acetate (10 mL). The organic layers were combined, dried over anhydrous sodium sulfate, and concentrated in vacuo. The residue was purified using a silica gel column (PE/EA=3/1) to afford the title compound as a brown solid. LC/MS m/z=429.1 [M+H]+.

후처리

  1. temperaturecooled to room temperature
  2. concentrationconcentrated
  3. extractionextracted with ethyl acetate (10 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe residue was purified

출처 및 근거

ORD 기록
ord-995fcf1c575142c48980d4d0ebfd214a
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403807B2

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