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

Hydrochloric Acid → 7-(4-hydroxybut-1-ynyl)-9,9-dimethyl-9H-fluoren-2-ol

HRID 511063
노트
인쇄 미리보기

반응식

HRID 511063 반응식
Br[C:2]1[CH:14]=[C:13]2[C:5]([C:6]3[CH:7]=[CH:8][C:9]([OH:17])=[CH:10][C:11]=3[C:12]2([CH3:16])[CH3:15])=[CH:4][CH:3]=1.[CH2:18]([OH:22])[CH2:19][C:20]#[CH:21].O.Cl>C1COCC1.C(NC(C)C)(C)C.Cl[Pd](Cl)([P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)[P](C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.[Cu]I>[OH:22][CH2:18][CH2:19][C:20]#[C:21][C:2]1[CH:14]=[C:13]2[C:5]([C:6]3[CH:7]=[CH:8][C:9]([OH:17])=[CH:10][C:11]=3[C:12]2([CH3:16])[CH3:15])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 135663-Butyn-1-OLHCID 667980237-bromo-9,9-dimethyl-9H-fluoren-2-ol

생성물 1

HCID 667982407-(4-hydroxybut-1-ynyl)-9,9-dimethyl-9H-fluoren-2-ol

시약·촉매·용매 4

HCID 24350Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI)
촉매
HCID 178418476HCID 178418476, 화합물촉매
HCID 7912Diisopropylamine용매
HCID 8028Tetrahydrofuran용매2회

실험 절차

14.7 g (0.048 mol) of 7-bromo-9,9-dimethyl-9H-fluoren-2-ol, 1.3 g (1.85 mmol) of bis(triphenylphosphine)palladium(II) chloride and 0.5 g (2.6 mmol) of copper(I) iodide are initially introduced in 200 ml of THF and 20 ml of diisopropylamine, and a solution of 9.5 ml (0.13 mmol) of but-3-yn-1-ol in 50 ml of THF is added over the course of 2 h under reflux. When the addition is complete, the batch is heated under reflux for a further 1 h, added to water, acidified using dil. hydrochloric acid and extracted three times with ethyl acetate. The combined org. phases are dried over sodium sulfate, and the solvent is removed in vacuo. Chromatography of the crude product on silica gel with toluene/ethyl acetate (4:1) gives 7-(4-hydroxybut-1-ynyl)-9,9-dimethyl-9H-fluoren-2-ol as colourless oil.

후처리

  1. temperatureunder reflux
  2. additionWhen the addition
  3. temperaturethe batch is heated
  4. temperatureunder reflux for a further 1 h
  5. extractionextracted three times with ethyl acetate
  6. dry with materialphases are dried over sodium sulfate
  7. customthe solvent is removed in vacuo

출처 및 근거

ORD 기록
ord-c36117577c0344748ce132549f5a10f9
출처 데이터셋
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09096795B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트