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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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3-Pyridinecarboxaldehyde → Pyridine, 3-(2,2-dibromoethenyl)-

HRID 1760
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HRID 1760 반응식
[Br:1][C:2]([Br:5])(Br)Br.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[N:25]1[CH:30]=[CH:29][CH:28]=[C:27]([CH:31]=O)[CH:26]=1>C(Cl)Cl>[Br:1][C:2]([Br:5])=[CH:31][C:27]1[CH:26]=[N:25][CH:30]=[CH:29][CH:28]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 103713-PyridinecarboxaldehydeHCID 11205Carbon tetrabromideHCID 11776Triphenylphosphine

생성물 1

HCID 11334526Pyridine, 3-(2,2-dibromoethenyl)-수율 70%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Tetrabromomethane (24.82 g, 0.747 mole) and triphenylphosphine (39.17 g, 0.149 mole) were stirred together in dry methylene chloride (100 mL) for 5 min. at 0° C. under a nitrogen atmosphere. To this mixture was added dropwise pyridine 3-carboxaldehyde (4 g, 0.0373 mole). The solution was then stirred for 45 min. at ambient temperature. The reaction mixture was extracted with aqueous 6N hydrochloric acid (3×25 mL), the aqueous layer basified with solid sodium bicarbonate to pH 8-9 and extracted with chloroform (4×25 mL). The combined organic liquours were dried over anhydrous sodium sulfate, filtered and concentrated on a rotary evaporator to give a dark colored syrup. The crude product was chromatographed on silica gel (70-230 mesh) with chloroform:methanol (95:5) as eluant, to afford a light yellow solid (5.0 g, 70%) which rapidly turned dark on standing.

후처리

  1. extractionThe reaction mixture was extracted with aqueous 6N hydrochloric acid (3×25 mL)
  2. extractionextracted with chloroform (4×25 mL)
  3. dry with materialThe combined organic liquours were dried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated on a rotary evaporator
  6. customto give a dark colored syrup
  7. customThe crude product was chromatographed on silica gel (70-230 mesh) with chloroform:methanol (95:5) as eluant

출처 및 근거

ORD 기록
ord-b463cdcceaba4202b2513724f75023cf
출처 데이터셋
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05726316

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