Sodium hydride → 2-Bromo-N-Methylsulfonylacetamide

HRID 863775ノート

反応式

HRID 863775 の反応式
[H-].[Na+].[CH3:3][S:4]([NH2:7])(=[O:6])=[O:5].[Br:8][CH2:9][C:10](Br)=[O:11]>O1CCCC1>[Br:8][CH2:9][C:10]([NH:7][S:4]([CH3:3])(=[O:6])=[O:5])=[O:11]

参加物

5

反応物 3

HCID 24758Sodium hydrideHCID 61147Bromoacetyl bromideHCID 72879Methanesulfonamide

生成物 1

HCID 2629442-Bromo-N-Methylsulfonylacetamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

Sodium hydride (1.68 g×60%) was added to a stirred solution of methanesulfonamide (2.0 g) in dry tetrahydrofuran (20 ml) at room temperature. The resulting solution was stirred at room temperature for 1 h, at which time it was treated with a solution of bromoacetyl bromide (4.2 g) in dry tetrahydrofuran (10 ml). After 1 h the solvent was removed under reduced pressure and the residue taken up in water and acidified to pH3. The acidic solution was extracted into ethyl acetate, dried (MgSO4), filtered and the solvent removed under reduced pressure. Recrystallisation from isopropanol afforded the product as white needles: mp 112°-114° C.

後処理

  1. customAfter 1 h the solvent was removed under reduced pressure
  2. extractionThe acidic solution was extracted into ethyl acetate
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customthe solvent removed under reduced pressure
  6. customRecrystallisation from isopropanol

出典と根拠

ORDレコード
ord-63d3edc4a693446d8c49bf12eb6aacc3
出典データセット
uspto-grants-1996_10
特許番号
US05561130

反応ノート

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