Water → 2-[p-(2,4-Dichlorobenzyl)-phenoxi]-propionic acid amide

HRID 371890

反応式

HRID 371890 の反応式
[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[CH2:4][C:5]1[CH:10]=[CH:9][C:8]([OH:11])=[CH:7][CH:6]=1.Br[CH:18]([CH3:22])[C:19]([NH2:21])=[O:20].C(=O)([O-])[O-].[K+].[K+].O>CN(C)C=O>[Cl:1][C:2]1[CH:15]=[C:14]([Cl:16])[CH:13]=[CH:12][C:3]=1[CH2:4][C:5]1[CH:6]=[CH:7][C:8]([O:11][CH:18]([CH3:22])[C:19]([NH2:21])=[O:20])=[CH:9][CH:10]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 1011182-BromopropanamideHCID 139387094-(2,4-Dichlorobenzyl)-phenol

生成物 1

HCID 706227402-[p-(2,4-Dichlorobenzyl)-phenoxi]-propionic acid amide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 25.3 g of 4-(2,4-dichlorobenzyl)-phenol and 15.2 g of α-bromopropionic acid amide in 100 ml of dimethyl formamide was stirred for 2 hours at 100° C together with 16 g of potassium carbonate. After cooling, the reaction mixture was poured into 1 liter of water. A viscous oil precipitated which was absorbed in methylene chloride and washed with water. After drying over sodium sulfate, the solvent was distilled off under reduced pressure. The remaining colorless crystals were recrystallized from methanol. Yield: 25.8 g; melting point 148° - 149° C. ##STR5##

後処理

  1. temperatureAfter cooling
  2. customA viscous oil precipitated which
  3. customwas absorbed in methylene chloride
  4. washwashed with water
  5. dry with materialAfter drying over sodium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe remaining colorless crystals were recrystallized from methanol

出典と根拠

ORDレコード
ord-5991b704c0034b9283fb1896623af89d
出典データセット
uspto-grants-1978_05
特許番号
US04088474

関連ノート

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