Water → HCID 21470465, 화합물

HRID 2294753노트

반응식

HRID 2294753 반응식
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

참가 물질

6

반응물 4

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

생성물 1

HCID 21470465HCID 21470465, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-9913ec651e9f423a947bb83c71eef2ac
출처 데이터셋
uspto-grants-1997_11
특허 번호
US05690909

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