Acetic Acid → 4-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde

HRID 369688

反応式

HRID 369688 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([O:23][CH2:24][CH:25]=[C:26]([Cl:28])[Cl:27])[CH:5]=[C:6]([Cl:22])[C:7]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14][CH:15](OCC)[O:16]CC.C(O)(=O)C.Cl>O>[Cl:1][C:2]1[CH:3]=[C:4]([O:23][CH2:24][CH:25]=[C:26]([Cl:28])[Cl:27])[CH:5]=[C:6]([Cl:22])[C:7]=1[O:8][CH2:9][CH2:10][CH2:11][CH2:12][O:13][CH2:14][CH:15]=[O:16]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 184293933,5-Dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene

生成物 1

HCID 538269084-(2,6-Dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)butyloxyacetaldehyde収率 98.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

First, 1.81 g of 3,5-dichloro-1-(3,3-dichloro-2-propenyloxy)-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene was added to a mixture of 10 ml of acetic acid and 1 ml of concentrated hydrochloric acid with stirring under ice cooling. After further stirring for 15 minutes, the reaction mixture was poured into water and extracted twice with diethyl ether. The diethyl ether layers were combined and washed with water, aqueous sodium hydrogencarbonate solution and then saturated sodium chloride solution. The combined diethyl ether layer was dried over magnesium sulfate, and the diethyl ether was distilled out, which afforded 1.51 g of 4-(2,6-dichloro-4-(3,3-dichloro-2-propenyloxy)phenoxy)-butyloxyacetaldehyde (yield, 94%).

後処理

  1. stirringAfter further stirring for 15 minutes
  2. extractionextracted twice with diethyl ether
  3. washwashed with water, aqueous sodium hydrogencarbonate solution
  4. dry with materialThe combined diethyl ether layer was dried over magnesium sulfate
  5. distillationthe diethyl ether was distilled out

出典と根拠

ORDレコード
ord-ff03748e3fd349718a22b40499543d59
出典データセット
uspto-grants-2000_10
特許番号
US06140274

関連ノート

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