1-Bromo-2-Chloroethane → HCID 86741981, 화합물

HRID 2414077노트

반응식

HRID 2414077 반응식
C([Li])CCC.C(NCC)C.[CH2:11]([CH:14]([CH2:17][CH2:18][CH3:19])[C:15]#[N:16])[CH2:12][CH3:13].Br[CH2:21][CH2:22][Cl:23]>CCCCCC.CCOCC.O>[Cl:23][CH2:22][CH2:21][C:14]([CH2:17][CH2:18][CH3:19])([CH2:11][CH2:12][CH3:13])[C:15]#[N:16]

참가 물질

8

반응물 4

HCID 78491-Bromo-2-ChloroethaneHCID 8021DiethylamineHCID 833302-PropylvaleronitrileHCID 178418339Butyllithium

생성물 1

HCID 86741981HCID 86741981, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 3283Diethyl Ether용매3회HCID 8058Hexane용매

실험 절차

To the solution (245 ml) of 1,6M n butyllithium in hexane is added, drop by drop in an atmosphere of nitrogen and with stirring, the solution of 28.8 g of diethylamine in 100 ml of anhydrous ether. After 1 hour, the solution of 49.2 g of 2-propyl pentane nitrile in 100 ml of anhydrous ether is added at ambient temperature then, after return to ambient temperature, the solution of 49.1 g of 1-bromo 2-chloro ethane in 700 ml of anhydrous ether is added. The mixture is taken to reflux for 15 hours then, whilst cooling the reaction mixture in an ice bath, water is added. The organic phase is separated, washed with water, then with a dilute solution of hydrochloric acid and again with water. It is dried over sodium sulfate and the solvent is evaporated. The residue is distilled and a liquid is obtained; b.p./20 mm Hg: 140°-150° C.

후처리

  1. temperatureto reflux for 15 hours
  2. temperaturewhilst cooling the reaction mixture in an ice bath
  3. customThe organic phase is separated
  4. washwashed with water
  5. dry with materialIt is dried over sodium sulfate
  6. customthe solvent is evaporated
  7. distillationThe residue is distilled
  8. customa liquid is obtained
  9. custom140°-150° C.

출처 및 근거

ORD 기록
ord-c1dc846746ee4ceabfa96141e679cd84
출처 데이터셋
uspto-grants-1988_01
특허 번호
US04721710

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