Ammonium Chloride → HCID 14851973, 화합물

HRID 1032714

반응식

HRID 1032714 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 14851973HCID 14851973, 화합물

시약·촉매·용매 2

HCID 1049Pyridine용매HCID 8028Tetrahydrofuran용매2회

반응 조건

온도
-40 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-597cc87d81364b66a4448ffc9aee34c3
출처 데이터셋
uspto-grants-1990_09
특허 번호
US04959363

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