Acetic Acid → 3-(2,2-Dichlorovinyloxy)-benzaldehyde

HRID 1578124ノート

反応式

HRID 1578124 の反応式
[Cl:1][C:2]([Cl:13])=[CH:3][O:4][C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][CH:12]=1)[CH2:8]Br.C1N2CN3CN(C2)CN1C3.C(O)(=[O:26])C>O>[Cl:1][C:2]([Cl:13])=[CH:3][O:4][C:5]1[CH:6]=[C:7]([CH:10]=[CH:11][CH:12]=1)[CH:8]=[O:26]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 4101HexamethylenetetramineHCID 204827061-(Bromomethyl)-3-[(2,2-dichloroethenyl)oxy]benzene

生成物 1

HCID 134899763-(2,2-Dichlorovinyloxy)-benzaldehyde

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 8.5 g of 3-(2,2-dichlorovinyloxy)-benzyl bromide in 12.6 ml of acetic acid and 12.6 ml of water are added 8.4 g of hexamethylene tetramine. The resultant solution is refluxed for two hours. Subsequently 10 ml of HC1 are added and the reaction mixture is stirred for half an hour at 100°-110° C. The solution is washed with 100 ml of water and extracted cold (3 times) with 100 ml of ethyl acetate. The extract is washed with sodium carbonate solution and evaporated, to yield 5.8 g of 3-(2,2-dichlorovinyloxy)-benzaldehyde as a yellowish-brown oil, which can be used without further purification.

後処理

  1. additionSubsequently 10 ml of HC1 are added
  2. washThe solution is washed with 100 ml of water
  3. extractionextracted cold (3 times) with 100 ml of ethyl acetate
  4. washThe extract is washed with sodium carbonate solution
  5. customevaporated

出典と根拠

ORDレコード
ord-7fe54801ba4f4bdbbb6f73b7ff4eab5f
出典データセット
uspto-grants-1981_09
特許番号
US04291056

反応ノート

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