Dimethylformamide → HCID 21833680、化合物

HRID 1418713ノート

反応式

HRID 1418713 の反応式
[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([OH:13])=[CH:9][CH:8]=2)[CH:5]=[CH:4][CH:3]=[N:2]1.Cl[CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O>[N:1]1([CH2:6][C:7]2[CH:12]=[CH:11][C:10]([O:13][CH2:15][C:16]([O:18][CH2:19][CH3:20])=[O:17])=[CH:9][CH:8]=2)[CH:5]=[CH:4][CH:3]=[N:2]1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7751Ethyl chloroacetateHCID 11430Potassium CarbonateHCID 1334121-(4-Hydroxybenzyl)pyrazole

生成物 1

HCID 21833680HCID 21833680、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
50 °C

実験手順

A mixture of 60 g of 4-(1-pyrazolyl)methylphenol, 54.9 g of ethyl chloroacetate, 95.1 g of potassium carbonate, and 500 ml of anhydrous dimethylformamide was heated at 50° C. under stirring for 5 hours, followed by cooling to room temperature. The reaction mixture was poured into 1 liter of water, which was extracted twice with 200 ml of ethyl acetate. The organic layers were combined, washed with water, saturated aqueous ammonium chloride solution and then saturated sodium chloride solution, dried with anhydrous magnesium sulfate, and concentrated under reduced pressure to give crude ethyl 4-(1-pyrazolyl)methylphenoxyacetate as an oil.

後処理

  1. temperatureby cooling to room temperature
  2. extractionwas extracted twice with 200 ml of ethyl acetate
  3. washwashed with water, saturated aqueous ammonium chloride solution
  4. dry with materialsaturated sodium chloride solution, dried with anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-2ab669d3ae454d618460604234aed81f
出典データセット
uspto-grants-1999_03
特許番号
US05883262

反応ノート

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