Phosphorus tribromide → 6-(1-Bromoethyl)-4,4-dimethylchroman

HRID 2118519

반응식

HRID 2118519 반응식
[CH3:1][C:2]1([CH3:15])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH:12](O)[CH3:13])[CH:10]=2)[O:5][CH2:4][CH2:3]1.P(Br)(Br)[Br:17]>CCOCC.N1C=CC=CC=1.CCCCCC>[CH3:1][C:2]1([CH3:15])[C:11]2[C:6](=[CH:7][CH:8]=[C:9]([CH:12]([Br:17])[CH3:13])[CH:10]=2)[O:5][CH2:4][CH2:3]1

참가 물질

6

반응물 2

HCID 24614Phosphorus tribromideHCID 140102484,4-Dimethyl-6-(1-hydroxyethyl)chroman

생성물 1

HCID 140102506-(1-Bromoethyl)-4,4-dimethylchroman수율 83.8%

시약·촉매·용매 3

HCID 1049Pyridine촉매HCID 3283Diethyl Ether용매HCID 8058Hexane용매2회

반응 조건

온도
0 °C

실험 절차

6.2 g of 4,4-dimethyl-6-(1-hydroxyethyl)chromane were dissolved in 3 ml of absolute ether and 20 ml of hexane and the solution was treated with 3 drops of pyridine. At a temperature of 0°-5° C. there was slowly added dropwise thereto a solution of 5.4 g of phosphorus tribromide in 20 ml of hexane. The mixture was stirred at 0° C. for a further 3 hours, poured onto ice and extracted with ether. The organic phase was washed with dilute sodium bicarbonate solution and water, dried over sodium sulphate and evaporated. There were obtained 4.5 g of 4,4-dimethyl-6-(1-bromoethyl)chromane in the form of a reddish oil which was converted into the phosphonium bromide without further purification.

후처리

  1. additionAt a temperature of 0°-5° C. there was slowly added dropwise
  2. additionpoured onto ice
  3. extractionextracted with ether
  4. washThe organic phase was washed with dilute sodium bicarbonate solution and water
  5. dry with materialdried over sodium sulphate
  6. customevaporated

출처 및 근거

ORD 기록
ord-b1566a18aafd4e60b56d5a61e499e417
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04678793

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