1,4-Bis(1,2-dibromoethyl)benzene → 1,4-Diethynylbenzene

HRID 1086788

반응식

HRID 1086788 반응식
Br[CH:2]([C:5]1[CH:10]=[CH:9][C:8]([CH:11](Br)[CH2:12]Br)=[CH:7][CH:6]=1)[CH2:3]Br.CC(C)([O-])C.[K+]>C(O)(C)(C)C>[C:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]#[CH:12])=[CH:7][CH:6]=1)#[CH:3]

참가 물질

4

반응물 2

HCID 970181,4-Bis(1,2-dibromoethyl)benzeneHCID 23665647Potassium tert-butoxide

생성물 1

HCID 1204631,4-Diethynylbenzene수율 79.9%

시약·촉매·용매 1

HCID 6386tert-Butanol용매

실험 절차

In a 2 liter-volume four-necked flask having the same equipments as used in 1) above were charged 100 g of 1,4-bis(1,2-dibromoethyl)benzene, 103 g of potassium t-butoxide and 1 liter of t-butyl alcohol, and the mixture was stirred taking care not to rapidly raise the temperature by cooling on an ice bath. The stirring was continued while gradually elevating the temperature finally to a refluxing temperature, at which stirring was conducted for 1.5 hours. The reaction mixture was poured into 6 liters of ice-water, and the thus formed precipitate was filtered by suction. Purification by sublimation (60°±3° C., 1 to 2 mmHg) gave 22.4 g of crystals of p-diethynylbenzene ##STR8## having a melting point of 96.5° C.

후처리

  1. temperatureto rapidly raise the temperature
  2. temperatureby cooling on an ice bath
  3. stirringat which stirring
  4. filtrationthe thus formed precipitate was filtered by suction
  5. customPurification by sublimation (60°±3° C., 1 to 2 mmHg)

출처 및 근거

ORD 기록
ord-a820d6d45f0b4a019b31ee3b25c40641
출처 데이터셋
uspto-grants-1991_07
특허 번호
US05032489

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