Hydrazine → HCID 15728745、化合物

HRID 1084766ノート

反応式

HRID 1084766 の反応式
[CH3:1][O:2][CH:3]([O:18][CH3:19])[C:4]1[CH:8]=[CH:7][S:6][C:5]=1[C:9](=O)[C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[F:16].[OH-].[K+].NN>C(O)CO>[CH3:19][O:18][CH:3]([O:2][CH3:1])[C:4]1[CH:8]=[CH:7][S:6][C:5]=1[CH2:9][C:10]1[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=1[F:16]

参加物

5

反応物 3

HCID 9321HydrazineHCID 14797Potassium HydroxideHCID 15728739HCID 15728739、化合物

生成物 1

HCID 15728745HCID 15728745、化合物

試薬・触媒・溶媒 1

HCID 174Ethylene Glycol溶媒

実験手順

To 2-(2-fluorobenzoyl)-3-thiophenecarboxaldehyde dimethylacetal (144 g), and ethylene glycol (500 ml) was added potassium hydroxide (115 g) and hydrazine.monohydrate (74.8 ml). The reaction mixture was warmed slowly in an oil bath to 70°-75° C.; 10-15 ml of distillate was collected. The temperature was slowly increased to 120°-125° C. and maintained at this temperature for 30 mins. The oil bath was removed, and the mixture allowed to cool to room temperature. Ether and water were added and the layers separated. The aqueous layer was extracted with ether-dichloromethane, and the combined organic layers washed with brine and dried over anhydrous potassium carbonate, filtered and concentrated. The residue in ethyl acetate was passed through a pad of silica gel and ethyl acetate. Concentration afforded 2-(2-fluorobenzyl)-3-thiophenecarboxaldehyde dimethylacetal.

後処理

  1. temperatureThe reaction mixture was warmed slowly in an oil bath to 70°-75° C.
  2. distillation10-15 ml of distillate was collected
  3. temperatureThe temperature was slowly increased to 120°-125° C.
  4. temperaturemaintained at this temperature for 30 mins
  5. customThe oil bath was removed
  6. additionEther and water were added
  7. customthe layers separated
  8. extractionThe aqueous layer was extracted with ether-dichloromethane
  9. washthe combined organic layers washed with brine
  10. dry with materialdried over anhydrous potassium carbonate
  11. filtrationfiltered
  12. concentrationconcentrated
  13. concentrationConcentration

出典と根拠

ORDレコード
ord-78b4759767df4680861c6a8c2dbc442b
出典データセット
uspto-grants-1991_04
特許番号
US05006536

反応ノート

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