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

HRID 1633739

反応式

HRID 1633739 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6393Carbon tetrafluoride溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d625cb0354ea4fdb9c0c5ba8db793974
出典データセット
uspto-grants-2003_01
特許番号
US06503998B2

関連ノート

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