Benzyl Bromide → 1-(Benzyloxy)-2,5-dibromo-4-(dodecyloxy)benzene

HRID 643182노트

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HRID 643182 반응식
[CH2:1](Br)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Br:9][C:10]1[CH:15]=[C:14]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:13]([Br:29])=[CH:12][C:11]=1[OH:30].C([O-])([O-])=O.[K+].[K+]>C(O)C>[Br:9][C:10]1[CH:15]=[C:14]([O:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH3:28])[C:13]([Br:29])=[CH:12][C:11]=1[O:30][CH2:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 667607252,5-Dibromo-4-(dodecyloxy)phenol

생성물 1

HCID 667610971-(Benzyloxy)-2,5-dibromo-4-(dodecyloxy)benzene수율 80%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
50 °C

실험 절차

Benzyl bromide (3.8 ml, 0.031 mol) was added drop wise to a stirred solution of 2,5-dibromo-4-dodecyloxy phenol (a) (6.95 g, 0.015 mol) and anhydrous K2CO3 (3.28 g, 0.023 mol) in 700 ml of absolute ethanol at 40-50° C. The reaction mixture was stirred for 10 h at 50° C., progress of the reaction was monitored using TLC, cooled to RT and evaporated to remove the solvent. An equal volume of distilled water was added to the residue and the mixture was stirred for one hour at 0° C. The resulting precipitate was collected by filtration, washed with water, and dried in vacuum. Recrystallization was done in methanol to get 80% yield.

후처리

  1. temperaturecooled to RT
  2. customevaporated
  3. customto remove the solvent
  4. additionAn equal volume of distilled water was added to the residue
  5. stirringthe mixture was stirred for one hour at 0° C
  6. filtrationThe resulting precipitate was collected by filtration
  7. washwashed with water
  8. customdried in vacuum
  9. customRecrystallization
  10. customto get 80% yield

출처 및 근거

ORD 기록
ord-df43d9c23ddd48e58fff5fa5dd126afd
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700040B2

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