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Imidazole → 3-{4-[(4-fluorobenzyl)oxy]phenyl}-N-(3-thioxo-3H-1,2,4-dithiazol-5-yl)acrylamide

HRID 1393852
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HRID 1393852 반응식
[F:1][C:2]1[CH:20]=[CH:19][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([CH:14]=[CH:15][C:16](O)=[O:17])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C(N1C=CN=C1)(N1C=CN=C1)=O.N1C=CN=C1.[H-].[Na+].[NH2:40][C:41]1[S:42][S:43][C:44](=[S:46])[N:45]=1>O1CCCC1.O>[F:1][C:2]1[CH:20]=[CH:19][C:5]([CH2:6][O:7][C:8]2[CH:13]=[CH:12][C:11]([CH:14]=[CH:15][C:16]([NH:40][C:41]3[S:42][S:43][C:44](=[S:46])[N:45]=3)=[O:17])=[CH:10][CH:9]=2)=[CH:4][CH:3]=1
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참가 물질

8

반응물 5

HCID 795Imidazole2회HCID 24758Sodium hydrideHCID 682631,1'-CarbonyldiimidazoleHCID 8053823-[4-[(4-fluorophenyl)methoxy]phenyl]prop-2-enoic AcidHCID 2735329Xanthane hydride

생성물 1

HCID 723564373-{4-[(4-fluorobenzyl)oxy]phenyl}-N-(3-thioxo-3H-1,2,4-dithiazol-5-yl)acrylamide
수율 9.4%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

3-{4-[(4-Fluorobenzyl)oxy]phenyl}acrylic acid (1.00 g, 3.67 mmol) was dissolved in tetrahydrofuran (11 ml), and 1,1′-carbonyldiimidazole (0.714 g, 4.40 mmol) was added thereto. The imidazole mixture was stirred for1 hour at room temperature. Sodium hydride (60% oil suspension 0.147 g, 3.67 mmol) was suspended in tetrahydrofuran (11 ml), and 3-amino-1,2,4-dithiazole-5-thione (0.552 g, 3.67 mmol) was added thereto. After being stirred for 30 minutes at 0° C., the reaction mixture, with the imidazole mixture added thereto, was stirred for 2 hours at room temperature. The mixture, with water added thereto, was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over MgSO4, and then concentrated. The obtained residue was purified by silica gel column chromatography (chloroform), to give 3-{4-[(4-fluorobenzyl)oxy]phenyl}-N-(3-thioxo-3H-1,2,4-dithiazol-5-yl)acrylamide (Compound 4) (0.139 g, 9%).

후처리

  1. stirringwas stirred for 2 hours at room temperature
  2. extractionwas extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated
  6. customThe obtained residue was purified by silica gel column chromatography (chloroform)

출처 및 근거

ORD 기록
ord-cb728f0938b645b9984a795aa0ad3dcc
출처 데이터셋
uspto-grants-2008_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07348017B2

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