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Triethylamine → 1,1,2,2,3,3-Hexafluorocyclopentane

HRID 1031788
ノート
印刷プレビュー

反応式

HRID 1031788 の反応式
Cl[C:2]1[C:6]([F:8])([F:7])[C:5]([F:10])([F:9])[C:4]([F:12])([F:11])[C:3]=1Cl.C(N(CC)CC)C>CO.[Ni]>[F:7][C:6]1([F:8])[CH2:2][CH2:3][C:4]([F:12])([F:11])[C:5]1([F:9])[F:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 8471TriethylamineHCID 128151,2-Dichloroperfluorocyclopentene

生成物 1

HCID 109975961,1,2,2,3,3-Hexafluorocyclopentane収率 60%

試薬・触媒・溶媒 2

HCID 935Nickel触媒HCID 887Methanol溶媒

実験手順

In a 1.3 l stainless steel autoclave, 245 g (1 mol) of 1,2-dichloro-3,3,4,4,5,5-hexafluorocyclopentene were hydrogenated at 60 to 70° C. with the addition of 202 g (2 mol) of triethylamine in 200 ml of methanol and in the presence of 20 g of Raney nickel. Over a period of 12 hours, the theoretical amount of hydrogen was absorbed at a hydrogen pressure of 40 to 50 bar. The reaction mixture was filtered and the methanolic solution was diluted with 400 ml of water. The lower organic phase was separated, washed with 100 ml of 5% aqueous hydrochloric acid, and dried over sodium sulfate. Distillation through a 1-m spinning band column gave 106 g (60% of theory) of 1,1,2,2,3,3-hexafluorocyclopentane having a boiling point of 87-88° C. at 1013 mbar. The mass spectrum showed the molecular ion at m/e 178.

後処理

  1. customthe theoretical amount of hydrogen was absorbed at a hydrogen pressure of 40 to 50 bar
  2. filtrationThe reaction mixture was filtered
  3. additionthe methanolic solution was diluted with 400 ml of water
  4. customThe lower organic phase was separated
  5. washwashed with 100 ml of 5% aqueous hydrochloric acid
  6. dry with materialdried over sodium sulfate
  7. distillationDistillation through a 1-m

出典と根拠

ORDレコード
ord-41d12da6e0404f15bf95a98cf19ae22f
出典データセット
uspto-grants-1990_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04954666

反応ノート

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