홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

3-Bromophenol → 3-(3,7-Dimethyloctyloxy)bromobenzene

HRID 990168
노트
인쇄 미리보기

반응식

HRID 990168 반응식
N[C@H](C(O)=O)CC1C=C2C(C=CC=C2)=CC=1.[OH-].[K+].[Br:19][C:20]1[CH:21]=[C:22]([OH:26])[CH:23]=[CH:24][CH:25]=1.[CH3:27][CH:28]([CH2:32][CH2:33][CH2:34][CH:35]([CH3:37])[CH3:36])[CH2:29][CH2:30]Cl>C(O)C>[CH3:27][CH:28]([CH2:32][CH2:33][CH2:34][CH:35]([CH3:37])[CH3:36])[CH2:29][CH2:30][O:26][C:22]1[CH:21]=[C:20]([Br:19])[CH:25]=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 115633-BromophenolHCID 14797Potassium Hydroxide2회HCID 1859152-NaphthylalanineHCID 2273601-Chloro-3,7-dimethyloctane

생성물 1

HCID 180041813-(3,7-Dimethyloctyloxy)bromobenzene

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

450 ml of ethanol were placed in the reaction vessel and admixed with Nal (10.5 g; 70 mmol) and KOH (67.3 g; 1.2 mol). A temperature rise from 25 to 40° C. was observed after addition of the KOH. After cooling to room temperature, 3-bromophenol (175.5 g; 1 mol) was added. The white suspension became beige during this addition. 3,7-dimethyloctyl chloride (186.32 g; 212.94 ml; 1.05 mol) was added over a period of 3 minutes by means of a dropping funnel. The mixture was stirred further for 2 hours at RT and subsequently for 96 hours at an internal temperature of 80° C. Ethanol was distilled off. The residue was taken up in ethyl acetate and the precipitate was separated off by filtration. The organic phase was extracted three times with 10% strength by weight aqueous NaOH solution, washed once with H2O, three times with H2O which had been acidified with CO2 and again with H2O. After drying over MgSO4, the solvent was again taken off on a rotary evaporator and the crude product was purified by fractional vacuum distillation.

후처리

  1. customfrom 25 to 40° C.
  2. additionThe white suspension became beige during this addition
  3. distillationEthanol was distilled off
  4. customthe precipitate was separated off by filtration
  5. extractionThe organic phase was extracted three times with 10% strength by weight aqueous NaOH solution
  6. washwashed once with H2O, three times with H2O which
  7. dry with materialAfter drying over MgSO4
  8. customthe solvent was again taken off on a rotary evaporator
  9. distillationthe crude product was purified by fractional vacuum distillation

출처 및 근거

ORD 기록
ord-cbc7c7afb4c94357abc088835cb8dc80
출처 데이터셋
uspto-grants-2002_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06458909B1

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트