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Dimethyloxostannane → HCID 178439146, 화합물

HRID 1297603
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HRID 1297603 반응식
[C:1]([C:3]([CH3:30])([CH3:29])[C:4]1[CH:27]=[CH:26][C:7]([CH2:8][NH:9][C:10](=[O:25])[C:11]2[CH:16]=[CH:15][CH:14]=[N:13][C:12]=2[O:17][C:18]2[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=2)=[C:6]([F:28])[CH:5]=1)#[N:2].[N:31]([Si](C)(C)C)=[N+:32]=[N-:33].C[Sn](=O)C>C1(C)C=CC=CC=1>[F:28][C:6]1[CH:5]=[C:4]([C:3]([CH3:30])([C:1]2[NH:33][N:32]=[N:31][N:2]=2)[CH3:29])[CH:27]=[CH:26][C:7]=1[CH2:8][NH:9][C:10](=[O:25])[C:11]1[CH:16]=[CH:15][CH:14]=[N:13][C:12]=1[O:17][C:18]1[CH:23]=[CH:22][C:21]([F:24])=[CH:20][CH:19]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 75277DimethyloxostannaneHCID 78378AzidotrimethylsilaneHCID 17832827N-[4-(Cyano-dimethyl-methyl)-2-fluoro-benzyl]-2-(4-fluoro-phenoxy)-nicotinamide

생성물 1

HCID 178439146HCID 178439146, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
100 °C

실험 절차

To N-[4-(cyano-dimethyl-methyl)-2-fluoro-benzyl]-2-(4-fluoro-phenoxy)-nicotinamide (2.36 g) in a 50 mL sealable tube were added anhydrous toluene (2 mL), azidotrimethylsilane (1.42 mL), and dimethyl tin oxide (0.19 g). The reaction was stirred at 100° C. for seven days. The solvent was removed in vacuo. The residue was then taken up in acetone, and the precipitate was filtered and rinsed with water, giving a brown solid (1.13 g). The filtrate was concentrated, then taken up in satd. aq. sodium bicarbonate, (50 mL) and washed with ethyl acetate (50 mL). The aqueous was acidified to pH 3, and extracted with ethyl acetate (3×100 mL). The combined organics were dried over magnesium sulfate, filtered, and concentrated in vacuo. The combined recovered solids were recrystallized with ethanol, yielding the title compound (1.26 g).

후처리

  1. customThe solvent was removed in vacuo
  2. filtrationthe precipitate was filtered
  3. washrinsed with water

출처 및 근거

ORD 기록
ord-577cf779f58d43839084f99b4bbe5267
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07250518B2

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