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1-(5-Chloro-2-methoxy-benzenesulfonyl)-piperazine → HCID 66801819, 화합물

HRID 528047
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HRID 528047 반응식
Cl[C:2]1[N:10]=[CH:9][N:8]=[C:7]2[C:3]=1[N:4]=[C:5]([C:12]1[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=1)[N:6]2[CH3:11].[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([O:34][CH3:35])=[C:23]([S:25]([N:28]2[CH2:33][CH2:32][NH:31][CH2:30][CH2:29]2)(=[O:27])=[O:26])[CH:24]=1>C(O)(C)C>[Cl:18][C:19]1[CH:20]=[CH:21][C:22]([O:34][CH3:35])=[C:23]([S:25]([N:28]2[CH2:29][CH2:30][N:31]([C:2]3[N:10]=[CH:9][N:8]=[C:7]4[C:3]=3[N:4]=[C:5]([C:12]3[CH:13]=[N:14][N:15]([CH3:17])[CH:16]=3)[N:6]4[CH3:11])[CH2:32][CH2:33]2)(=[O:26])=[O:27])[CH:24]=1
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참가 물질

4

반응물 2

HCID 10713391-(5-Chloro-2-methoxy-benzenesulfonyl)-piperazineHCID 86711714HCID 86711714, 화합물

생성물 1

HCID 66801819HCID 66801819, 화합물수율 49%

시약·촉매·용매 1

HCID 3776Isopropanol용매

실험 절차

A stirred solution of 6-chloro-9-methyl-8-(1-methyl-1H-pyrazol-4-yl)-9H-purine (30 mg, 0.12 mmol), 1-(5-chloro-2-methoxyphenylsulfonyl)piperazine (43.6 mg, 0.15 mmol, Oakwood Products, Inc.), and triethylaminem (84.0 uL, 0.60 mmol) in isopropyl alcohol (2.0 mL) were heated to 80° C. for 16 hours. The resulting precipitate was collected by vacuum filtration, washed with ethanol (2 mL), water (2 mL) and diethyl ether (2 mL) and dried under reduced pressure, to give 29.6 mg (49% yield) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ 8.43 (s, 1H), 8.23 (s, 1H), 8.05 (s, 1H), 7.70 (dt, 2H), 7.27 (d, 1H), 3.95 (s, 3H), 3.88 (s, 3H), 3.83 (s, 3H), 3.31-3.25 (m, 4H). MS (EI) for C21H23ClN8O3S: 503.7 (MH+).

후처리

  1. filtrationThe resulting precipitate was collected by vacuum filtration
  2. washwashed with ethanol (2 mL), water (2 mL) and diethyl ether (2 mL)
  3. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-f996ba4dcc114270a2a0b3e4352e679d
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09346807B2

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