Carbon Tetrachloride → 1,5-Bis(chloromethyl)-2,4-di(propan-2-yl)benzene

HRID 846877

反応式

HRID 846877 の反応式
[Sn](Cl)(Cl)(Cl)Cl.C(O[CH2:9][Cl:10])C.[CH:11]([C:14]1[CH:19]=[CH:18][CH:17]=[C:16]([CH:20]([CH3:22])[CH3:21])[CH:15]=1)([CH3:13])[CH3:12].[C:23](Cl)(Cl)(Cl)[Cl:24]>>[Cl:24][CH2:23][C:17]1[CH:18]=[C:19]([CH2:9][Cl:10])[C:14]([CH:11]([CH3:13])[CH3:12])=[CH:15][C:16]=1[CH:20]([CH3:22])[CH3:21]

参加物

5

反応物 4

HCID 5943Carbon TetrachlorideHCID 74501,3-DiisopropylbenzeneHCID 18523Chloromethyl ethyl ether2 回HCID 24287Tin tetrachloride2 回

生成物 1

HCID 148505431,5-Bis(chloromethyl)-2,4-di(propan-2-yl)benzene

反応条件

温度
0 °C

実験手順

55 ml (0.46 mol) of tin tetrachloride are added dropwise with cooling in an ice bath (exothermic reaction) to a solution of 230 ml (2.43 mol) of chloromethyl ethyl ether and 197 g (1.22 mol) of 1,3-diisopropylbenzene in 600 ml of carbon tetrachloride and the mixture is stirred at 0° C. for 1 h. After stirring overnight at +25° C., 142 g (1.5 mol) of chloromethyl ethyl ether and 74 ml (0.46 mol) of tin tetrachloride are again added dropwise at 0° C. and the mixture is stirred overnight at +25° C. The reaction mixture is added to ice/hydrochloric acid, and the organic phase is separated off, washed with water and dried using sodium sulphate. After concentrating, the residue is taken up with petroleum ether, filtered through 1 kg of silica gel (230-400 mesh) and distilled in a high vacuum.

後処理

  1. temperaturewith cooling in an ice bath
  2. stirringAfter stirring overnight at +25° C.
  3. stirringthe mixture is stirred overnight at +25° C
  4. customthe organic phase is separated off
  5. washwashed with water
  6. customdried
  7. concentrationAfter concentrating
  8. filtrationfiltered through 1 kg of silica gel (230-400 mesh)
  9. distillationdistilled in a high vacuum

出典と根拠

ORDレコード
ord-1b88865d09304a0d95c270c7508e6ee6
出典データセット
uspto-grants-1992_08
特許番号
US05138090

関連ノート

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