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

HRID 342648

반응식

HRID 342648 반응식
[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]

참가 물질

5

반응물 2

HCID 24408BromineHCID 825294-Methylsulfonylacetophenone

생성물 1

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

시약·촉매·용매 2

HCID 176Acetic Acid용매2회HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9c90ca2f589e4b9f9840497f897d634c
출처 데이터셋
uspto-grants-1999_01
특허 번호
US05859036

연결된 노트

불러오는 중…