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Hexane → HCID 15289933、化合物

HRID 1975706
ノート
印刷プレビュー

反応式

HRID 1975706 の反応式
[Cl:1][C:2]1[CH:14]=[CH:13][CH:12]=[CH:11][C:3]=1[CH2:4][C:5]1[O:10][CH2:9][CH2:8][O:7][N:6]=1.[Br:15]N1C(=O)CCC1=O.C(OCC)(=O)C.CCCCCC>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Cl:1][C:2]1[CH:14]=[CH:13][CH:12]=[CH:11][C:3]=1[CH:4]([Br:15])[C:5]1[O:10][CH2:9][CH2:8][O:7][N:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 8058HexaneHCID 8857Ethyl AcetateHCID 67184N-bromobutanimideHCID 14879552HCID 14879552、化合物

生成物 1

HCID 15289933HCID 15289933、化合物収率 87%

試薬・触媒・溶媒 2

HCID 7187Benzoyl Peroxide触媒
HCID 5943
Carbon Tetrachloride
溶媒

実験手順

4.0 g (19 mmole) of 3-(2-chlorobenzyl)-5,6-dihydro-1,4,2-dioxazine (prepared as described in Preparation 1) were dissolved in 40 ml of carbon tetrachloride, and then 4.1 g (23 mmole) of N-bromosuccinimide and 0.2 g of benzoyl peroxide were added to the solution, which was then stirred, whilst heating, for 8 hours. At the end of this time, 100 ml of ethyl acetate and 100 ml of hexane were added to the solution, and the mixture was stirred at room temperature for 30 minutes; insolubles were then removed by filtration. The filtrate was concentrated by evaporation under reduced pressure, to give 4.8 g of the title compound as a yellow oil.

後処理

  1. temperaturewhilst heating, for 8 hours
  2. stirringthe mixture was stirred at room temperature for 30 minutes
  3. custominsolubles were then removed by filtration
  4. concentrationThe filtrate was concentrated by evaporation under reduced pressure

出典と根拠

ORDレコード
ord-db1856477e9e4c9ba559e754190def51
出典データセット
uspto-grants-1994_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05288726

反応ノート

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