Water → HCID 21470465、化合物

HRID 2294753ノート

反応式

HRID 2294753 の反応式
ClC1C=CC=C(C(OO)=[O:9])C=1.O.[F:13][C:14]([F:27])([F:26])[C:15]([C:22]([F:25])([F:24])[F:23])([C:18]([F:21])([F:20])[F:19])[CH:16]=[CH2:17].C(=O)(O)[O-].[Na+]>C(OCC)C>[F:13][C:14]([F:26])([F:27])[C:15]([C:18]([F:21])([F:20])[F:19])([C:22]([F:23])([F:24])[F:25])[CH:16]1[O:9][CH2:17]1

参加物

6

反応物 4

HCID 962WaterHCID 70297m-Chloroperbenzoic acidHCID 516892Sodium BicarbonateHCID 27826293,3,3-Tris(trifluoromethyl)-1-propene

生成物 1

HCID 21470465HCID 21470465、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

32.9 g (105 mmol) of 3-chloroperbenzoic acid with a peracid content of 55% is added in portions with stirring and cooling with water to a solution of 24.6 g (100 mmol) of 4,4,4-trifluoro-3,3-bis(trifluoromethyl)-but-1-ene in 150 ml of absolute diethyl ether. After addition is completed, it is refluxed for 3 hours. It is allowed to cool, and the solution is stirred in cold, saturated sodium bicarbonate solution. The ethereal solution is separated, washed with sodium chloride solution, dried on sodium sulfate and concentrated by evaporation on a column. The residue is purified by bulb tube distillation (vacuum 30 mbar, 130° C. bath).

後処理

  1. additionAfter addition
  2. temperatureit is refluxed for 3 hours
  3. temperatureto cool
  4. customThe ethereal solution is separated
  5. washwashed with sodium chloride solution
  6. customdried on sodium sulfate
  7. concentrationconcentrated by evaporation on a column
  8. customThe residue is purified by bulb tube
  9. distillationdistillation (vacuum 30 mbar, 130° C. bath)

出典と根拠

ORDレコード
ord-9913ec651e9f423a947bb83c71eef2ac
出典データセット
uspto-grants-1997_11
特許番号
US05690909

反応ノート

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