Bromoform → HCID 53803475, 화합물

HRID 1196173

반응식

HRID 1196173 반응식
[CH3:1][C:2]([CH3:11])=[CH:3][CH2:4][CH2:5][C:6]([OH:10])([C:8]#[CH:9])[CH3:7].[CH:12]([Br:15])(Br)[Br:13].[OH-].[Na+]>[Cl-].C([N+](CC)(CC)CC1C=CC=CC=1)C>[Br:13][C:12]1([Br:15])[C:2]([CH3:1])([CH3:11])[CH:3]1[CH2:4][CH2:5][C:6]([CH3:7])([OH:10])[C:8]#[CH:9]

참가 물질

5

반응물 3

HCID 5558Bromoform2회HCID 14798Sodium HydroxideHCID 62842Dehydrolinalool

생성물 1

HCID 53803475HCID 53803475, 화합물수율 84.5%

시약·촉매·용매 1

HCID 66133Benzyl triethylammonium chloride촉매2회

실험 절차

Dehydrolinalool (60.8 g, 0.4 mol), bromoform (151.6 g, 0.6 mol) and 0.8 g of triethylbenzylammonium chloride are placed in a reaction flask and 64 g of a 50% sodium hydroxide solution are added during 30 minutes. The reaction is exothermic and the mixture is therefore cooled with ice. After stirring the mixture at room temperature for 21.5 hours the same amounts of bromoform and triethylbenzylammonium chloride are again added. The reaction becomes exothermic and is cooled with ice. The mixture is left to react at 0° for a further 4 hours, poured onto ice and extracted with methylene chloride. The organic phases are washed neutral, dried and evaporated. In this manner there are obtained 109.5 g (84%) of 5-(2'2'-dibromo-3'3'-dimethylcyclopropyl)-3-methyl-1-pentyn-3-ol.

후처리

  1. temperaturethe mixture is therefore cooled with ice
  2. additionare again added
  3. temperatureis cooled with ice
  4. waitThe mixture is left
  5. customto react at 0° for a further 4 hours
  6. additionpoured onto ice
  7. extractionextracted with methylene chloride
  8. washThe organic phases are washed neutral
  9. customdried
  10. customevaporated

출처 및 근거

ORD 기록
ord-d0890348fa134590832f593206ada504
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05113021

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