Iodine → HCID 18541883、化合物

HRID 1777563ノート

反応式

HRID 1777563 の反応式
[I:1]I.[F:3][C:4]1[CH:5]=[C:6]([CH:8]=[C:9]([F:12])[C:10]=1[F:11])[NH2:7]>C(O)C.S([O-])([O-])(=O)=O.[Ag+2]>[F:3][C:4]1[C:5]([I:1])=[C:6]([CH:8]=[C:9]([F:12])[C:10]=1[F:11])[NH2:7]

参加物

5

反応物 2

HCID 807IodineHCID 27249913,4,5-Trifluoroaniline

生成物 1

HCID 18541883HCID 18541883、化合物収率 42%

試薬・触媒・溶媒 2

HCID 178418844HCID 178418844、化合物触媒HCID 702Ethanol溶媒

実験手順

Iodine (0.621 g; 2.45 mmol) was added to a stirred mixture of silver sulphate (0.763 g; 2.45 mmol) and 3,4,5-trifluoroaniline (0.360 g; 2.45 mmol) in ethanol (5 mL). The reaction mixture was then stirred at room temperature for 18 hours and filtered over celite. The volatiles were removed under reduced pressure and the residue was partitioned between ethyl acetate and a saturated aqueous solution of sodium thiosulfate. The organic layer was washed with brine, dried and concentrated under reduced pressure. The crude residue was purified by flash chromatography on silica gel (eluent 2 to 40% ethyl acetate in heptane) to afford 0.279 g (42%) of the title compound as a white solid.

後処理

  1. filtrationfiltered over celite
  2. customThe volatiles were removed under reduced pressure
  3. customthe residue was partitioned between ethyl acetate
  4. washThe organic layer was washed with brine
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customThe crude residue was purified by flash chromatography on silica gel (eluent 2 to 40% ethyl acetate in heptane)

出典と根拠

ORDレコード
ord-30f237e4b8b54fbc964b81450bd51f4d
出典データセット
uspto-grants-2016_02
特許番号
US09266832B2

反応ノート

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