Benzyltrimethylammonium hydroxide → HCID 86734504, 화합물

HRID 436395

반응식

HRID 436395 반응식
[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[CH:4]=1)=[CH2:2].[OH-:16].C([N+](C)(C)C)C1C=CC=CC=1>N1C=CC=CC=1>[CH:1]([C:3]1[C:4](=[O:16])[C:5]2[C:13](=[CH:14][CH:15]=1)[C:12]1[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=1)[CH:6]=2)=[CH2:2]

참가 물질

4

반응물 2

HCID 66854Benzyltrimethylammonium hydroxideHCID 110416072-ethenyl-9H-fluorene

생성물 1

HCID 86734504HCID 86734504, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매2회

반응 조건

온도
0 °C

실험 절차

The 2-vinylfluorene prepared in Example I is dissolved in 800 milliliters of pyridine and cooled to 0° C. One-half milliliter of a 40% solution of benzyltrimethyl ammonium hydroxide in pyridine is slowly added with air being bubbled through the reaction solution. The initially formed red coloration fades over a period of 1 to 2 hours and the solution is poured into water and extracted with benzene to yield 9 grams (90% theory) of a yellow solid. The residue is chromatographed on alumina (Woehlm basic) and eluted with benzene. Recrystallization from hexane gives 2-vinylfluorenone as a pale yellow material (melting point 69°-70° C). The structure of the product is confirmed by nuclear magnetic resonance and elemental analysis.

후처리

  1. custombeing bubbled through the reaction solution
  2. additionthe solution is poured into water
  3. extractionextracted with benzene
  4. customto yield 9 grams (90% theory) of a yellow solid
  5. customThe residue is chromatographed on alumina (Woehlm basic)
  6. washeluted with benzene
  7. customRecrystallization from hexane

출처 및 근거

ORD 기록
ord-66c6e7d151874e6e90a58a75dec0020c
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04009151

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