Benzoyl Peroxide → 4-[(6-Acetoxyhexyl)sulfonyl]benzyl bromide

HRID 1633739

반응식

HRID 1633739 반응식
[C:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][S:11]([C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][CH:15]=1)(=[O:13])=[O:12])(=[O:3])[CH3:2].[Br:21]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(F)(F)(F)F>[C:1]([O:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][S:11]([C:14]1[CH:19]=[CH:18][C:17]([CH2:20][Br:21])=[CH:16][CH:15]=1)(=[O:13])=[O:12])(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 7187Benzoyl PeroxideHCID 67184N-bromobutanimideHCID 186800254-[(6-Acetoxyhexyl)sulfonyl]toluene

생성물 1

HCID 186800214-[(6-Acetoxyhexyl)sulfonyl]benzyl bromide수율 71%

시약·촉매·용매 1

HCID 6393Carbon tetrafluoride용매

실험 절차

2.0 g of 4-[(6-acetoxyhexyl)sulfonyl]toluene, 1.3 g of N-bromo-succinimide (NBS), 0.015 g of benzoyl peroxide (BPO) , and 20 mL of carbon tetrafluoride were added to a 250 mL round bottomed flask and heated with reflux for 12 hours in nitrogen. The mixture was allowed to cool down and then filtered. The filtrate was washed by deionized water repeatedly. The organic fraction was dried over anhydrous magnesium sulfate and then concentrated by a rotary evaporator. The concentrate was further purified by re-crystallization to produce a white solid. The yield was 71% with the following structure.

후처리

  1. temperatureheated
  2. temperaturewith reflux for 12 hours in nitrogen
  3. temperatureto cool down
  4. filtrationfiltered
  5. washThe filtrate was washed by deionized water repeatedly
  6. dry with materialThe organic fraction was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated by a rotary evaporator
  8. customThe concentrate was further purified by re-crystallization
  9. customto produce a white solid

출처 및 근거

ORD 기록
ord-d625cb0354ea4fdb9c0c5ba8db793974
출처 데이터셋
uspto-grants-2003_01
특허 번호
US06503998B2

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