Isobutylene → HCID 23330246, 화합물

HRID 224759노트

반응식

HRID 224759 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 23330246HCID 23330246, 화합물

시약·촉매·용매 1

HCID 8078Cyclohexane용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-77b2b95aaede44cab24a6058d1da66d5
출처 데이터셋
uspto-grants-1980_11
특허 번호
US04234517

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