Sodium Iodide → N-(2,2,3,3,4,4,4-heptafluorobutyl)-5-iodo-N-methylpentanesulfonamide

HRID 742953ノート

反応式

HRID 742953 の反応式
[I-:1].[Na+].Cl[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][S:9]([N:12]([CH2:14][C:15]([F:24])([F:23])[C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[F:18])[CH3:13])(=[O:11])=[O:10]>C(C(C)=O)C>[F:23][C:15]([F:24])([C:16]([F:22])([F:21])[C:17]([F:20])([F:19])[F:18])[CH2:14][N:12]([CH3:13])[S:9]([CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][I:1])(=[O:11])=[O:10]

参加物

4

反応物 2

HCID 5238Sodium IodideHCID 197110325-chloro-N-(2,2,3,3,4,4,4-heptafluorobutyl)-N-methyl-pentanesulfonamide

生成物 1

HCID 19711036N-(2,2,3,3,4,4,4-heptafluorobutyl)-5-iodo-N-methylpentanesulfonamide収率 96.6%

試薬・触媒・溶媒 1

HCID 6569Methyl Ethyl Ketone溶媒

実験手順

300 mg of sodium iodide were added to a solution of 355 mg of the product of Step A in 3 ml of methyl ethyl ketone and the mixture was refluxed for 4 hours. After evaporation of the solvent, the residue was taken up in water and extracted with ethyl acetate. The extracts were washed with an aqueous solution of sodium thiosulfate, then of sodium chloride, and evaporated to dryness under reduced pressure to obtain 425 mg of the expected product in the form of a colourless oil which slowly crystallized.

後処理

  1. temperaturethe mixture was refluxed for 4 hours
  2. customAfter evaporation of the solvent
  3. extractionextracted with ethyl acetate
  4. washThe extracts were washed with an aqueous solution of sodium thiosulfate
  5. customof sodium chloride, and evaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-4b22165e5e3a483394309476474b57c8
出典データセット
uspto-grants-1996_09
特許番号
US05556845

反応ノート

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