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Di-tert-butyl peroxide → HCID 10466935、化合物

HRID 1838684
ノート
印刷プレビュー

反応式

HRID 1838684 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 8033Di-tert-butyl peroxideHCID 27788772-Bromopentafluoropropene2 回

生成物 1

HCID 10466935HCID 10466935、化合物収率 26%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-0834ab4eab9e42d593473c3a39313a4d
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06673976B1

反応ノート

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