Bromine → 2-Bromo-4'-(methylsulfonyl)acetophenone

HRID 342648

反応式

HRID 342648 の反応式
[Br:1]Br.[CH3:3][S:4]([C:7]1[CH:12]=[CH:11][C:10]([C:13](=[O:15])[CH3:14])=[CH:9][CH:8]=1)(=[O:6])=[O:5]>C(O)(=O)C.Cl>[Br:1][CH2:14][C:13]([C:10]1[CH:11]=[CH:12][C:7]([S:4]([CH3:3])(=[O:5])=[O:6])=[CH:8][CH:9]=1)=[O:15]

参加物

5

反応物 2

HCID 24408BromineHCID 825294-Methylsulfonylacetophenone

生成物 1

HCID 7358232-Bromo-4'-(methylsulfonyl)acetophenone

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒2 回HCID 313Hydrochloric Acid溶媒

実験手順

38.5 ml of bromine dissolved in 110 ml of acetic acid are added dropwise onto a suspension of 159 g of the product of Example 1 in 1.6 l of acetic acid and 1.6 ml of hydrochloric acid, the reaction mixture is then stirred for 3 h at ambient temperature. The precipitate obtained is filtered, rinsed with water and then dissolved in dichloromcthane and dried over magnesium sulphate. The dichloromethane is evaporated off, the residue is taken up in pentane and filtered to give 100 g of the expected product. A second batch is obtained by pouring the filtrate of the reaction mixture onto an icc/water mixture, then by filtering off and by treating the precipitate as previously. The two batches are then combined and recrystallised from acetic acid.

後処理

  1. customThe precipitate obtained
  2. filtrationis filtered
  3. washrinsed with water
  4. dissolutiondissolved in dichloromcthane
  5. dry with materialdried over magnesium sulphate
  6. customThe dichloromethane is evaporated off
  7. filtrationfiltered

出典と根拠

ORDレコード
ord-9c90ca2f589e4b9f9840497f897d634c
出典データセット
uspto-grants-1999_01
特許番号
US05859036

関連ノート

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