Methanesulfonamide → 5-Bromo-N-methanesulfonylpentanamide

HRID 561772

反応式

HRID 561772 の反応式
[CH3:1][S:2]([NH2:5])(=[O:4])=[O:3].[Br:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11](Cl)=[O:12]>C(OCC)(=O)C>[Br:6][CH2:7][CH2:8][CH2:9][CH2:10][C:11]([NH:5][S:2]([CH3:1])(=[O:4])=[O:3])=[O:12]

参加物

4

反応物 2

HCID 72879MethanesulfonamideHCID 5211735-Bromovaleryl chloride

生成物 1

HCID 202961415-Bromo-N-methanesulfonylpentanamide収率 88.3%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

反応条件

温度
87.5 °C

実験手順

A mixture consisting of methanesulfonamide (4.76 g) and 5-bromovaleric acid chloride (10 g) was heated at 85-90° C. for one hour, was cooled to room temperature, and was diluted with ethyl acetate (75 mL). The solution was washed with water, brine, and dried over sodium sulfate. The solution was filtered and evaporated to 40 mL of solvent, then cooled to −15° C. A white precipitate formed, which was collected by filtration to afford the title intermediate (11.4 g, 88%) as a white solid; melting point 98-100° C.

後処理

  1. temperaturewas cooled to room temperature
  2. washThe solution was washed with water, brine
  3. dry with materialdried over sodium sulfate
  4. filtrationThe solution was filtered
  5. customevaporated to 40 mL of solvent
  6. temperaturecooled to −15° C
  7. customA white precipitate formed
  8. filtrationwhich was collected by filtration

出典と根拠

ORDレコード
ord-4ccd0fc749d9494d93f44d84999ebb6f
出典データセット
uspto-grants-2011_11
特許番号
US08063240B2

関連ノート

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