Boron tribromide → HCID 59611582、化合物

HRID 2039301ノート

反応式

HRID 2039301 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]3[CH:13]=[C:14]([O:17]C)[CH:15]=[CH:16][C:10]=3[CH:9]=2)=[CH:4][CH:3]=1.B(Br)(Br)Br>>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[S:12][C:11]3[CH:13]=[C:14]([OH:17])[CH:15]=[CH:16][C:10]=3[CH:9]=2)=[CH:4][CH:3]=1

参加物

3

反応物 2

HCID 25134Boron tribromideHCID 167197572-(4-Bromophenyl)-6-methoxybenzo[b]thiophene

生成物 1

HCID 59611582HCID 59611582、化合物収率 88%

実験手順

To a stirred solution of 2-(4-bromo-phenyl)-6-methoxy-benzo[b]thiophene (80 mg, 0.25 mmol) was added BBr3 (0.5 mL of 1 M in DCM, 0.5 mmol) at 0° C. The mixture was stirred for 3 hours at ambient temperature. DCM was removed under vacuum, and the residue was dissolved in ethyl acetate (30 mL) The organic layer was washed with NaHCO3 solution, water and brine, dried over Na2SO4, filtered and concentrated in vacuo. The obtained residue was treated with hexane to give the product (67 mg, 88%). m/z 303.0, 305.0 (M−H)−.

後処理

  1. customDCM was removed under vacuum
  2. dissolutionthe residue was dissolved in ethyl acetate (30 mL) The organic layer
  3. washwas washed with NaHCO3 solution, water and brine
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. additionThe obtained residue was treated with hexane

出典と根拠

ORDレコード
ord-b9c6915fa93e4c7b923f67ec13d56bf2
出典データセット
uspto-grants-2013_11
特許番号
US08575118B2

反応ノート

読み込み中…