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Dimethylformamide → 2,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)benzenamine

HRID 463452
ノート
印刷プレビュー

反応式

HRID 463452 の反応式
CN(C)C=O.Cl.[NH2:7][C:8]1[C:13]([Cl:14])=[CH:12][C:11]([OH:15])=[C:10]([Cl:16])[CH:9]=1.[OH-].[K+].[F:19][C:20]([F:24])=[C:21]([F:23])[F:22]>O>[Cl:14][C:13]1[CH:12]=[C:11]([O:15][C:21]([F:23])([F:22])[CH:20]([F:24])[F:19])[C:10]([Cl:16])=[CH:9][C:8]=1[NH2:7]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 8301TetrafluoroethyleneHCID 14797Potassium HydroxideHCID 135172884-Amino-2,5-dichlorophenol hydrochloride

生成物 1

HCID 135172892,5-Dichloro-4-(1,1,2,2-tetrafluoroethoxy)benzenamine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
85 °C

実験手順

A mixture of 100 ml dimethylformamide (DMF), 75 g (0.035 mole) 4-amino-2,5-dichlorophenol, hydrochloride, and 3.0 g (0.05 mole) KOH (pellets ground to powder) was placed in a 500 ml 3-necked round bottom flask fitted with a mechanical stirrer, thermometer and reflux condenser and was stirred for about 1 hour. It was then heated to 85° C. with stirring and 6.0 g (0.06 mole) of tetrafluoroethylene was bubbled in while heating at 85°-90° C. The addition took about 10 minutes. The reactor and contents were cooled in an ice water bath and 200 ml of water were added. The product was extracted with 200 ml methylene chloride and then again with 100 ml methylene chloride. The extracts were combined and the solvents removed by vacuum distillation. A residue (7 g) remained.

後処理

  1. customwas placed in a 500 ml 3-necked round bottom flask
  2. customfitted with a mechanical stirrer
  3. temperaturethermometer and reflux condenser
  4. stirringwith stirring
  5. temperaturewhile heating at 85°-90° C
  6. additionThe addition
  7. waittook about 10 minutes
  8. temperatureThe reactor and contents were cooled in an ice water bath
  9. extractionThe product was extracted with 200 ml methylene chloride
  10. customthe solvents removed by vacuum distillation

出典と根拠

ORDレコード
ord-987540b5256b4e5b9ac74ffb1b84ae6a
出典データセット
uspto-grants-1985_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04518804

反応ノート

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