Trifluoromethanesulfonic anhydride → HCID 59611359、化合物

HRID 1185961ノート

反応式

HRID 1185961 の反応式
[O:1]([S:9]([C:12]([F:15])([F:14])[F:13])(=[O:11])=[O:10])S(C(F)(F)F)(=O)=O.[Br:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[S:27][C:26]3[CH:28]=[C:29](O)[CH:30]=[CH:31][C:25]=3[CH:24]=2)=[CH:19][CH:18]=1>N1C=CC=CC=1>[Br:16][C:17]1[CH:22]=[CH:21][C:20]([C:23]2[S:27][C:26]3[CH:28]=[C:29]([O:1][S:9]([C:12]([F:13])([F:14])[F:15])(=[O:10])=[O:11])[CH:30]=[CH:31][C:25]=3[CH:24]=2)=[CH:19][CH:18]=1

参加物

4

反応物 2

HCID 67749Trifluoromethanesulfonic anhydrideHCID 59611582HCID 59611582、化合物

生成物 1

HCID 59611359HCID 59611359、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Tf2O was added slowly to a mixture of 2-(4-bromo-phenyl)-benzo[b]thiophen-6-ol (200 mg, 0.66 mol) in pyridine (3 mL) at 0° C. with stirring. The mixture was stirred at ambient temperature for 16 hours before quenched with NaHCO3 solution. The mixture was extracted with ethyl acetate (50 mL). The organic layer was washed with water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was used for next step reaction without further purification.

後処理

  1. stirringThe mixture was stirred at ambient temperature for 16 hours
  2. custombefore quenched with NaHCO3 solution
  3. extractionThe mixture was extracted with ethyl acetate (50 mL)
  4. washThe organic layer was washed with water and brine
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe obtained residue was used for next step reaction without further purification

出典と根拠

ORDレコード
ord-72b2cd99442c4c80b27c3dae71651241
出典データセット
uspto-grants-2014_03
特許番号
US08669234B2

反応ノート

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