Chlorosulfonic acid → HCID 59759968、化合物

HRID 1693138ノート

反応式

HRID 1693138 の反応式
[F:1][C:2]1[CH:14]=[CH:13][C:5]2[S:6][CH:7]=[C:8]([CH2:9][CH:10]([CH3:12])[CH3:11])[C:4]=2[CH:3]=1.[Cl:15][S:16](O)(=[O:18])=[O:17]>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:14]=[CH:13][C:5]2[S:6][C:7]([S:16]([Cl:15])(=[O:18])=[O:17])=[C:8]([CH2:9][CH:10]([CH3:11])[CH3:12])[C:4]=2[CH:3]=1

参加物

4

反応物 2

HCID 24638Chlorosulfonic acidHCID 597599805-Fluoro-3-isobutyl-benzo[b]thiophene

生成物 1

HCID 59759968HCID 59759968、化合物収率 60.5%

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

To a solution of 5-fluoro-3-isobutyl-benzo[b]thiophene 0.55 g) in chloroform (10 ml) was added chlorosulfonic acid (1.54 g), and the resulting mixture was stirred at rt for 3 h, quenched with ice/water, and extracted with methylene chloride. The organic phases were washed with water and aqueous sodium bicarbonate solution, dried and concentrated. The residue was chromatographed on silica gel using heptane/ethyl acetate as eluent to obtain the title compound (0.49 g) as a colorless oil. MS (EI): 306.8 (M)

後処理

  1. customquenched with ice/water
  2. extractionextracted with methylene chloride
  3. washThe organic phases were washed with water and aqueous sodium bicarbonate solution
  4. customdried
  5. concentrationconcentrated
  6. customThe residue was chromatographed on silica gel

出典と根拠

ORDレコード
ord-35f862ec1db543008e6a499e0857a2f9
出典データセット
uspto-grants-2012_04
特許番号
US08158655B2

反応ノート

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