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Di-tert-butyl peroxide → HCID 10466935, 화합물

HRID 1838684
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HRID 1838684 반응식
[C:1]([O:5]OC(C)(C)C)(C)(C)C.[C:11]([C:15](=[C:17]([F:19])[F:18])[Br:16])([F:14])([F:13])[F:12]>CO>[C:11]([CH:15]([C:17]([CH2:1][OH:5])([F:19])[F:18])[Br:16])([F:14])([F:13])[F:12]
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참가 물질

4

반응물 2

HCID 8033Di-tert-butyl peroxideHCID 27788772-Bromopentafluoropropene2회

생성물 1

HCID 10466935HCID 10466935, 화합물수율 26%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

In a quartz photochemical reaction vessel equipped with a dry ice condenser, a stirred mixture of methanol (20 g), ditert-butyl peroxide (0.79) and CF3C(Br)═CF2 (10 g, 0.05 mol), was irradiated at 254 nm for ˜6 hr at ambient temperature for under nitrogen. (Note: CF3CBr═CF2 was added as a liquid (BP, 24-25° C.) in one lot before the reaction). Then the reaction mixture was concentrated to remove excess methanol. The concentrated material was taken in ˜40 mL ether, washed with 20 ml 20% aqueous sodium bisulphite followed by brine (10 mL) and distilled to afford the CF3CHBrCF2CH2OH (2.0 g) as a colorless liquid. Yield=26% based on CF3CBr═CF2. Boiling point, 30-31° C./ 8-10 mm Hg. GC-MS: m/e at (C4H4BrF5O) for M+; NMR spectra are consistent with the structure.

후처리

  1. customIn a quartz photochemical reaction vessel equipped with a dry ice condenser
  2. customwas irradiated at 254 nm for ˜6 hr at ambient temperature for under nitrogen
  3. concentrationThen the reaction mixture was concentrated
  4. customto remove excess methanol
  5. washwashed with 20 ml 20% aqueous sodium bisulphite
  6. distillationdistilled

출처 및 근거

ORD 기록
ord-0834ab4eab9e42d593473c3a39313a4d
출처 데이터셋
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06673976B1

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