Hydrochloric Acid → HCID 54346943、化合物

HRID 1065603ノート

反応式

HRID 1065603 の反応式
[BH4-].[Na+].[Cl:3][C:4]1[C:5]([F:16])=[C:6]([C:10]([F:15])=[C:11]([Cl:14])[C:12]=1[F:13])[C:7](F)=[O:8].O.Cl>O1CCOCC1>[Cl:3][C:4]1[C:5]([F:16])=[C:6]([C:10]([F:15])=[C:11]([Cl:14])[C:12]=1[F:13])[CH2:7][OH:8]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 198504823,5-Dichloro-2,4,6-trifluorobenzoyl fluoride

生成物 1

HCID 54346943HCID 54346943、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

反応条件

温度
20 °C

実験手順

400 ml of dry dioxane and 55 g of sodium borohydride are initially introduced into a 2 l three-necked flask with a stirrer, reflux condenser and dropping funnel at 20° C., and 247 g of 3,5-dichloro-2,4,6-trifluorobenzoyl fluoride, dissolved in 250 ml of dry dioxane, are then added dropwise at this temperature. When the addition has ended, the mixture is stirred at 20° C. for a further 2 hours and then warmed to the reflux temperature for 1 hour. The solution is cooled to room temperature, a total of 50 ml of water are then added dropwise and the mixture is subsequently rendered acid with dilute hydrochloric acid. The reaction mixture is extracted three times with methylene chloride and, after drying the organic phase over sodium sulphate, the solvent is distilled off. 196.5 g (85% of the theoretical yield) of 3,5-dichloro-2,4,6-trifluorobenzyl alcohol of boiling point 134° to 135° C./20 mbars and melting point 67° to 68° C. are obtained from the residue by further distillation.

後処理

  1. temperaturereflux condenser
  2. customat 20° C.
  3. additionare then added dropwise at this temperature
  4. additionWhen the addition
  5. temperaturewarmed to the reflux temperature for 1 hour
  6. temperatureThe solution is cooled to room temperature
  7. extractionThe reaction mixture is extracted three times with methylene chloride
  8. dry with materialafter drying the organic phase over sodium sulphate
  9. distillationthe solvent is distilled off

出典と根拠

ORDレコード
ord-666aa7aec3a74cdba2fbc0354c04de4b
出典データセット
uspto-grants-1982_05
特許番号
US04330366

反応ノート

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