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Sodium hydride → 4-(3,4-Dihydro-2H-chromen-4-yloxy)-N,N,1,2-tetramethyl-1H-benzimidazole-6-carboxamide

HRID 2238579
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HRID 2238579 반응식
[OH:1][C:2]1[C:10]2[N:9]=[C:8]([CH3:11])[N:7]([CH3:12])[C:6]=2[CH:5]=[C:4]([C:13]([N:15]([CH3:17])[CH3:16])=[O:14])[CH:3]=1.[H-].[Na+].Cl[CH:21]1[C:30]2[C:25](=[CH:26][CH:27]=[CH:28][CH:29]=2)[O:24][CH2:23][CH2:22]1>CN(C)C=O>[O:24]1[C:25]2[C:30](=[CH:29][CH:28]=[CH:27][CH:26]=2)[CH:21]([O:1][C:2]2[C:10]3[N:9]=[C:8]([CH3:11])[N:7]([CH3:12])[C:6]=3[CH:5]=[C:4]([C:13]([N:15]([CH3:16])[CH3:17])=[O:14])[CH:3]=2)[CH2:22][CH2:23]1
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참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 127921574-ChlorochromanHCID 534710164-Hydroxy-N,N,1,2-tetramethyl-1H-benzimidazole-6-carboxamide

생성물 1

HCID 593038964-(3,4-Dihydro-2H-chromen-4-yloxy)-N,N,1,2-tetramethyl-1H-benzimidazole-6-carboxamide수율 52.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

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온도
70 °C

실험 절차

To a stirred suspension of 4-hydroxy-N,N,1,2-tetramethyl-1H-benzimidazole-6-carboxamide (50 mg, 0.21 mmol, WO 2004054984) in N,N-dimethylformamide (2 mL) was added sodium hydride (60% dispersion in mineral oil, 11 mg, 0.27 mmol) at room temperature. After stirring for 20 minutes, a solution of 4-chlorochromane (71 mg, 0.42 mmol, WO 2000078751) in N,N-dimethylformamide (1 mL) was added at room temperature. The reaction mixture was warmed to 70° C., and stirred for 6 hours at the same temperature. The reaction mixture was quenched with sodium hydrogencarbonate aqueous solution, and extracted with ethyl acetate (20 mL×2). The combined extracts were washed with water and brine, dried over magnesium sulfate, and concentrated in vacuum. The residue was purified by column chromatography on silica gel (ethyl acetate:methanol=10:1 as an eluent) to afford the title compound as a white solid (40 mg, 52%):

후처리

  1. stirringstirred for 6 hours at the same temperature
  2. customThe reaction mixture was quenched with sodium hydrogencarbonate aqueous solution
  3. extractionextracted with ethyl acetate (20 mL×2)
  4. washThe combined extracts were washed with water and brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in vacuum
  7. customThe residue was purified by column chromatography on silica gel (ethyl acetate

출처 및 근거

ORD 기록
ord-6b7509b4db3a4ce399f3008ddcf73e92
출처 데이터셋
uspto-grants-2010_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07718809B2

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