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Pyridine → HCID 67174946、化合物

HRID 1256065
ノート
印刷プレビュー

反応式

HRID 1256065 の反応式
[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[S:11](Cl)(=[O:13])=[O:12].[NH2:15][C:16]1[C:17]([F:26])=[CH:18][C:19]2[CH2:23][O:22][B:21]([OH:24])[C:20]=2[CH:25]=1.N1C=CC=CC=1>C(#N)C>[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[CH:4][C:3]=1[S:11]([NH:15][C:16]1[C:17]([F:26])=[CH:18][C:19]2[CH2:23][O:22][B:21]([OH:24])[C:20]=2[CH:25]=1)(=[O:13])=[O:12]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 24901388HCID 24901388、化合物HCID 457914292-Fluoro-4-nitrobenzenesulphonyl chloride

生成物 1

HCID 67174946HCID 67174946、化合物収率 89.3%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To a stirred solution of 2-fluoro-4-nitrobenzene-1-sulfonyl chloride (1.336 g, 5.57 mmol) and 6-amino-5-fluorobenzo[c][1,2]oxaborol-1(3H)-ol (0.93 g, 5.57 mmol) in 20 mL of ACN was added pyridine (900 uL, 11.14 mmol) dropwise. The reaction mixture was stirred at room temperature for 16 hours. After quenched with water, the solvent was removed in vacuo. The residue was extracted with ethyl acetate three times, and washed with water and brine. The organic layer was dried over Na2SO4, and concentrated to give 1.84 g of the title compound as a yellow residue. MS calcd for (C13H9BF2N2O6S): 370.0. MS found (ESI negative): (M−H)−=368.9

後処理

  1. customAfter quenched with water
  2. customthe solvent was removed in vacuo
  3. extractionThe residue was extracted with ethyl acetate three times
  4. washwashed with water and brine
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-cf4455bd13754ee084cbe367d8d039b4
出典データセット
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08461134B2

反応ノート

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