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P-Anisidine → HCID 53345317, 화합물

HRID 1464992
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HRID 1464992 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:20])[NH:9][C:10]2[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:19])([F:18])[F:17])[CH:11]=2)=[CH:4][C:3]=1[NH:21][C:22]([C:24]1[C:28]2[N:29]=[CH:30][N:31]=[C:32](S(C)=O)[C:27]=2[S:26][CH:25]=1)=[O:23].CCN(C(C)C)C(C)C.[CH3:45][O:46][C:47]1[CH:52]=[CH:51][C:50]([NH2:53])=[CH:49][CH:48]=1>O1CCOCC1.C(OCC)(=O)C>[CH3:45][O:46][C:47]1[CH:52]=[CH:51][C:50]([NH:53][C:32]2[C:27]3[S:26][CH:25]=[C:24]([C:22]([NH:21][C:3]4[CH:4]=[C:5]([C:8](=[O:20])[NH:9][C:10]5[CH:15]=[CH:14][CH:13]=[C:12]([C:16]([F:18])([F:19])[F:17])[CH:11]=5)[CH:6]=[CH:7][C:2]=4[CH3:1])=[O:23])[C:28]=3[N:29]=[CH:30][N:31]=2)=[CH:49][CH:48]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 7732P-AnisidineHCID 81531DiisopropylethylamineHCID 68263099HCID 68263099, 화합물

생성물 1

HCID 53345317HCID 53345317, 화합물수율 81%

시약·촉매·용매 2

HCID 8857Ethyl Acetate용매HCID 312751,4-Dioxane용매

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온도
120 °C

실험 절차

N-(2-methyl-5-(3-(trifluoromethyl)phenylcarbamoyl)phenyl)-4-(methylsulfinyl)thieno[3,2-d]pyrimidine-7-carboxamide (30 mg, 0.060 mmol) was dissolved in dioxane (1 mL) and DIPEA (20 μL, 0.119 mmol) and 4-methoxybenzeneamine (37 mg, 0.298 mmol) were added thereto. The reaction mixture was stirred at 120° C. for 18 hours, cooled to room temperature, diluted with ethyl acetate and washed with a brine. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure. The resulting mixture was purified by silica gel chromatography to obtain the title compound (28 mg, 81% yield).

후처리

  1. temperaturecooled to room temperature
  2. washwashed with a brine
  3. dry with materialThe organic layer was dried with MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting mixture was purified by silica gel chromatography

출처 및 근거

ORD 기록
ord-6143811d065547b2996062ae851c79dc
출처 데이터셋
uspto-grants-2015_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08999973B2

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