Ethylene Glycol → 2-[(3,5-Dichloro-6-fluoropyridin-2-yl)oxy]ethan-1-ol

HRID 1448407

反応式

HRID 1448407 の反応式
[Cl:1][C:2]1[C:3]([F:10])=[N:4][C:5](F)=[C:6]([Cl:8])[CH:7]=1.[OH-].[Na+].O.[CH2:14]([OH:17])[CH2:15][OH:16]>>[Cl:8][C:6]1[C:5]([O:16][CH2:15][CH2:14][OH:17])=[N:4][C:3]([F:10])=[C:2]([Cl:1])[CH:7]=1

参加物

5

反応物 4

HCID 174Ethylene Glycol2 回HCID 962WaterHCID 14798Sodium HydroxideHCID 6432773,5-Dichloro-2,6-difluoropyridine

生成物 1

HCID 203795872-[(3,5-Dichloro-6-fluoropyridin-2-yl)oxy]ethan-1-ol

実験手順

To a solution of 12 grams (0.065 mole) of 3,5-dichloro-2,6-difluoropyridine in 35 milliliters of ethylene glycol was added over a 10 minute period 2.7 grams of anhydrous sodium hydroxide in 40 milliliters of ethylene glycol. The reaction mixture was maintained at ~70° C. with agitation for 10 minutes, cooled and poured into water. The insoluble material is removed by filtration and the filtrate extracted with methylene chloride and dried. The solid 2-(3,5-dichloro-6-fluoro-2-pyridyloxy) ethanol product was crystallized from hexane and recovered in a yield of 9 grams (61 percent of theoretical). The product melted at 65°-67° C. and was found by analysis to have carbon, hydrogen, chlorine and nitrogen contents of 37.4, 3.1, 31.5 and 6.4 percent, respectively, as compared with the theoretical contents of 37.2, 2.7, 31.4 and 6.2 percent, respectively, calculated for the above-named compound.

後処理

  1. temperatureThe reaction mixture was maintained at ~70° C. with agitation for 10 minutes
  2. temperaturecooled
  3. customThe insoluble material is removed by filtration
  4. extractionthe filtrate extracted with methylene chloride
  5. customdried
  6. customThe solid 2-(3,5-dichloro-6-fluoro-2-pyridyloxy) ethanol product was crystallized from hexane
  7. customrecovered in a yield of 9 grams (61 percent of theoretical)

出典と根拠

ORDレコード
ord-5789e819244d4b7b9bd9c07fed8cc13b
出典データセット
uspto-grants-1979_12
特許番号
US04180395

関連ノート

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