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Hexane → 5-bromo-3-[1-(2,6-dichloro-3-fluorophenyl)-2-fluoro-2,2-bis(phenylsulfonyl)ethyl]-1H-pyrrolo[2,3-b]pyridine

HRID 2095743
ノート
印刷プレビュー

反応式

HRID 2095743 の反応式
[F:1][CH:2]([S:12]([C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)(=[O:14])=[O:13])[S:3]([C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1)(=[O:5])=[O:4].[Li]CCCC.CCCCCC.[Br:32][C:33]1[CH:34]=[C:35]2[C:41]([CH:42]([C:44]3[C:49]([Cl:50])=[CH:48][CH:47]=[C:46]([F:51])[C:45]=3[Cl:52])O)=[CH:40][NH:39][C:36]2=[N:37][CH:38]=1.S(Cl)(Cl)=O>C1COCC1.C(Cl)Cl>[C:15]1([S:12]([C:2]([S:3]([C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=2)(=[O:5])=[O:4])([F:1])[CH:42]([C:41]2[C:35]3[C:36](=[N:37][CH:38]=[C:33]([Br:32])[CH:34]=3)[NH:39][CH:40]=2)[C:44]2[C:49]([Cl:50])=[CH:48][CH:47]=[C:46]([F:51])[C:45]=2[Cl:52])(=[O:14])=[O:13])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 8058HexaneHCID 24386Thionyl ChlorideHCID 16079185Fluorobis(phenylsulfonyl)methaneHCID 67004517(5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)(2,6-dichloro-3-fluorophenyl)methanolHCID 178418339Butyllithium

生成物 1

HCID 86659327
5-bromo-3-[1-(2,6-dichloro-3-fluorophenyl)-2-fluoro-2,2-bis(phenylsulfonyl)ethyl]-1H-pyrrolo[2,3-b]pyridine

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-78 °C

実験手順

To a stirred solution of 1-(fluoro(phenylsulfonyl)methylsulfonyl)benzene (836 mg, 2.66 mmol) in THF (8.0 mL) was added 2.5 M of n-BuLi in Hexane (1.18 mL, 2.95 mmol) at −78° C.; the resulting mixture was stirred for 30 min at −78° C. before use. To a stirred solution of (5-bromo-1H-pyrrolo[2,3-b]pyridin-3-yl)-(2,6-dichloro-3-fluorophenyl)methanol (250.0 mg, 0.6410 mmol) in THF (5.0 mL, 62 mmol) was added thionyl chloride (0.12 mL, 1.6 mmol) at 0° C. The resulting mixture was stirred for 30 min at rt, then the solvent was removed and the residue was dried under high vacuum. To this residue was added THF (10.0 mL) followed by adding the previously prepared solution (lithiated 1-(fluoro(phenylsulfonyl)methylsulfonyl)benzene) by canula at −78° C. The resulting mixture was allowed to warm up to rt in about 1 hr. Then the solvent was removed under reduced pressure to give a residue, which was diluted by DCM and extracted by DCM (20 mL×3). The organic phase were combined, dried (Na2SO4) and concentrated to give a crude residue, which was purified by silica gel chromatography (eluent: 20% AcOEt in DCM) to give the title compound. MS (ES+): m/z 684.92, 686.92, 688.92 [MH+]. HPLC: tR=1.65 min (polar—3 min, TOF)

後処理

  1. stirringThe resulting mixture was stirred for 30 min at rt
  2. customthe solvent was removed
  3. customthe residue was dried under high vacuum
  4. additionTo this residue was added THF (10.0 mL)
  5. additionby adding the previously prepared solution (lithiated 1-(fluoro(phenylsulfonyl)methylsulfonyl)benzene) by canula at −78° C
  6. temperatureto warm up to rt in about 1 hr
  7. customThen the solvent was removed under reduced pressure
  8. customto give a residue, which
  9. extractionextracted by DCM (20 mL×3)
  10. dry with materialdried (Na2SO4)
  11. concentrationconcentrated
  12. customto give a crude residue, which
  13. customwas purified by silica gel chromatography (eluent: 20% AcOEt in DCM)

出典と根拠

ORDレコード
ord-ec6cab6a8c9d42d3abfde4f98b7e2bbe
出典データセット
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08445510B2

反応ノート

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