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

HRID 371890

반응식

HRID 371890 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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##

후처리

  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

출처 및 근거

ORD 기록
ord-5991b704c0034b9283fb1896623af89d
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04088474

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