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Water → HCID 178444243, 화합물

HRID 2259536
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HRID 2259536 반응식
[CH2:1]([C@H:6]1[CH2:11][CH2:10][C@H:9]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:8][CH2:7]1)[CH2:2][CH2:3][CH2:4][CH3:5].[Br:18]Br.O.S([O-])(O)=O.[Na+]>ClCCl.[Fe].II>[Br:18][C:15]1[CH:14]=[CH:13][C:12]([C@H:9]2[CH2:8][CH2:7][C@H:6]([CH2:1][CH2:2][CH2:3][CH2:4][CH3:5])[CH2:11][CH2:10]2)=[CH:17][CH:16]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 962WaterHCID 24408BromineHCID 23665763Sodium BisulfiteHCID 178444301HCID 178444301, 화합물

생성물 1

HCID 178444243HCID 178444243, 화합물수율 32.2%

시약·촉매·용매 3

HCID 807Iodine촉매
HCID 23925
Iron
촉매
HCID 6344Dichloromethane용매2회

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온도
-10 °C

실험 절차

In 30 ml of dichloromethane was dissolved 11.1 g of trans-4-pentylcyclohexylbenzene, and 0.1 g of iron powder and 0.05 g of iodine were added thereto. To the mixture was added dropwise 7.7 g of bromine dissolved in 20 ml of dichloromethane at 0° C. or lower. The mixture was stirred at -10° C. for 6 hours and then allowed to warm to room temperature. Water and then an aqueous solution of sodium hydrogensulfite were added to the reaction mixture, and the product was extracted with hexane. The extract was washed successively with a sodium bicarbonate aqueous solution, water and a saturated sodium chloride aqueous solution, and dried. The solvent was removed by distillation, and the resulting crude crystals were recrystallized from ethanol to give 4.8 g of 1-bromo-4-(trans-4-pentylcyclohexyl)benzene.

후처리

  1. additionwere added
  2. temperatureto warm to room temperature
  3. extractionthe product was extracted with hexane
  4. washThe extract was washed successively with a sodium bicarbonate aqueous solution, water
  5. dry with materiala saturated sodium chloride aqueous solution, and dried
  6. customThe solvent was removed by distillation
  7. customthe resulting crude crystals were recrystallized from ethanol

출처 및 근거

ORD 기록
ord-7e8eca7e02184be28eed3a5b90d3f58c
출처 데이터셋
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05474707

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