Isobutylene → HCID 23330246、化合物

HRID 224759ノート

反応式

HRID 224759 の反応式
[CH3:1][C:2](=[CH2:4])[CH3:3].[Cl:5][C:6]([Cl:13])([Cl:12])[CH2:7][CH2:8][C:9](Cl)=[O:10].C(N(CC)CC)C>C1CCCCC1>[Cl:5][C:6]([Cl:13])([Cl:12])[CH2:7][CH:8]1[C:2]([CH3:4])([CH3:3])[CH2:1][C:9]1=[O:10]

参加物

5

反応物 3

HCID 8255IsobutyleneHCID 8471TriethylamineHCID 545309984,4,4-Trichlorobutanoyl chloride

生成物 1

HCID 23330246HCID 23330246、化合物

試薬・触媒・溶媒 1

HCID 8078Cyclohexane溶媒2 回

実験手順

261 g of isobutylene is injected into a 1 liter autoclave containing 49 g (0.23 mol) of 4,4,4-trichlorobutyric acid chloride in 280 ml of cyclohexane. A solution of 28.3 g (0.28 mol) of triethylamine in 233 ml of cyclohexane is pumped in at 70° C. in the course of 4 hours. The reaction mixture is afterwards held at 70° C. for a further 4 hours. The precipitated hydrochloride of the triethylamine is filtered off; the filtrate obtained is washed with dilute hydrochloric acid and then with water, dried over sodium sulphate and concentration by evaporation. Distillation of the residue yields 2-(2',2',2'-trichloroethyl)-3,3-dimethylcyclobutanone as a clear liquid, b.p. 118°-122° C./14 mm Hg.

後処理

  1. customis pumped in at 70° C. in the course of 4 hours
  2. filtrationThe precipitated hydrochloride of the triethylamine is filtered off
  3. customthe filtrate obtained
  4. washis washed with dilute hydrochloric acid
  5. dry with materialwith water, dried over sodium sulphate and concentration by evaporation
  6. distillationDistillation of the residue

出典と根拠

ORDレコード
ord-77b2b95aaede44cab24a6058d1da66d5
出典データセット
uspto-grants-1980_11
特許番号
US04234517

反応ノート

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