Ammonium Chloride → HCID 14851973、化合物

HRID 1032714

反応式

HRID 1032714 の反応式
[CH3:1][C:2]([CH3:7])([CH3:6])[C:3](Cl)=[O:4].[F:8][C:9]1[CH:14]=[C:13](Cl)[CH:12]=[CH:11][C:10]=1[CH3:16].[Mg].[Cl-].[NH4+:19]>O1CCCC1.N1C=CC=CC=1>[F:8][C:9]1[CH:14]=[C:13]([CH:9]2[CH:14]=[CH:13][N:19]([C:3](=[O:4])[C:2]([CH3:7])([CH3:6])[CH3:1])[CH:11]=[CH:10]2)[CH:12]=[CH:11][C:10]=1[CH3:16]

参加物

7

反応物 4

HCID 25517Ammonium ChlorideHCID 62493Pivaloyl chlorideHCID 5206304-Chloro-2-fluorotolueneHCID 5462224Magnesium

生成物 1

HCID 14851973HCID 14851973、化合物

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-40 °C

実験手順

To a solution of 45 ml pyridine in 800 ml tetrahydrofuran (THF) was added dropwise 50 ml trimethylacetyl chloride. The mixture was stirred 3 hrs. at room temperature, 4.0 g cuprous iodide was added, and the mixture stirred for 1 hr. longer. The mixture was then cooled to -40° C. and a Grignard reagent prepared from 45 ml 2-fluoro-4-chlorotoluene and 10 g magnesium in 300 ml THF was added dropwise The reaction mixture was stirred overnight at room temperature, ammonium chloride solution added, and the product was extracted and isolated to give 90 g of an oil used directly in the next reaction.

後処理

  1. stirringthe mixture stirred for 1 hr
  2. additionwas added dropwise The reaction mixture
  3. stirringwas stirred overnight at room temperature
  4. extractionthe product was extracted
  5. customisolated

出典と根拠

ORDレコード
ord-597cc87d81364b66a4448ffc9aee34c3
出典データセット
uspto-grants-1990_09
特許番号
US04959363

関連ノート

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