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

Water → 9,9-Dibutyl-2-nitro-9H-fluorene

HRID 630643
노트
인쇄 미리보기

반응식

HRID 630643 반응식
[N+:1]([C:4]1[CH:16]=[CH:15][C:14]2[C:13]3[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=3)[CH2:7][C:6]=2[CH:5]=1)([O-:3])=[O:2].[OH-].[K+].[I-].[K+].O>CS(C)=O>[CH2:16]([C:7]1([CH2:7][CH2:8][CH2:9][CH3:10])[C:6]2[CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:16]=[CH:15][C:14]=2[C:13]2[C:8]1=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:4][CH2:5][CH3:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 4875Potassium IodideHCID 118312-NitrofluoreneHCID 14797Potassium Hydroxide

생성물 1

HCID 444715309,9-Dibutyl-2-nitro-9H-fluorene수율 158.7%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
15 °C

실험 절차

12.66 g of 2-nitrofluorene (1) (60 mmol), 21.0 g of potassium hydroxide (0.3 mol, purity: 80%), and 1.01 g of potassium iodide (6 mmol) were dissolved in 200 ml of anhydrous dimethylsulfoxide under nitrogen atmosphere, and a reaction temperature was maintained at 15° C. Then, 33 ml of n-bromobutane (0.3 mol) was slowly added thereto for 2 hours, followed by stirring at 15° C. for 1 hour. Thereafter, 200 ml of distilled water was added to the reaction mixture and stirred for about 30 minutes, a product was extracted with 300 ml of dichloromethane, and the extracted organic layer was washed with 100 ml of distilled water three times. Then, the recovered organic layer was dried over anhydrous magnesium sulfate, and the solvent was distilled under reduced pressure. The obtained product was purified using a silica gel column chromatography (eluent: dichloromethane:n-hexane=20:1), thereby obtaining 15.4 g of 9,9-di-n-butyl-2-nitrofluorene (5) (79.5%) as a light yellow product.

후처리

  1. stirringstirred for about 30 minutes
  2. extractiona product was extracted with 300 ml of dichloromethane
  3. washthe extracted organic layer was washed with 100 ml of distilled water three times
  4. dry with materialThen, the recovered organic layer was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled under reduced pressure
  6. customThe obtained product was purified

출처 및 근거

ORD 기록
ord-146d8a8000824b8cb558b0638bf11f17
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09316906B2

반응 노트

불러오는 중…

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트