1H-Indole, 4,5,6,7-tetrafluoro- → Indole

HRID 1352185

반응식

HRID 1352185 반응식
O.O=[Al]O[Al]=O.O=[Si]=O.F[C:11]1[C:19](F)=[C:18](F)[C:17](F)=[C:16]2[C:12]=1[CH:13]=[CH:14][NH:15]2>CC1C=CC=CC=1C>[NH:15]1[C:16]2[C:12](=[CH:11][CH:19]=[CH:18][CH:17]=2)[CH:13]=[CH:14]1

참가 물질

4

반응물 2

HCID 1400511H-Indole, 4,5,6,7-tetrafluoro-HCID 517273Quaternium 18-bentonite

생성물 1

HCID 798Indole수율 90%

시약·촉매·용매 1

HCID 7237O-Xylene용매2회

반응 조건

온도
100 °C

실험 절차

In the drybox, to a 250 ml round bottom flask was added the TEAL-treated Benclay (10.390 g, as described in 1-2) and 100 mL of anhydrous o-xylene. To the stirred slurry was added an o-xylene solution of 4,5,6,7-tetrafluoroindole (1.891 g, 0.010 mole). After stirring for 15 minutes, the stirring was stopped and the reaction mixture was heated to 100° C. During this time, the reaction mixture was stirred periodically for 1-2 minutes every 15-20 minutes. After the first 30 minutes at 100° C., the color of the solution turns from colorless to golden yellow. The reaction mixture was allowed to cool to room temperature and collected by vacuum filtration to give a yellow (golden) solid and a pale yellow solution. The solid was washed with toluene (3×50 mL) and dried in vacuo for ˜15 hours. Indole-modified clay samples were recovered in >90% yield and stored in the drybox freezer (−35° C.) until they were to be used.

후처리

  1. stirringDuring this time, the reaction mixture was stirred periodically for 1-2 minutes every 15-20 minutes
  2. customAfter the first 30 minutes
  3. customat 100° C.
  4. temperatureto cool to room temperature
  5. filtrationcollected by vacuum filtration
  6. customto give a yellow (golden) solid
  7. washThe solid was washed with toluene (3×50 mL)
  8. customdried in vacuo for ˜15 hours
  9. customIndole-modified clay samples were recovered in >90% yield
  10. customstored in the drybox freezer (−35° C.) until they

출처 및 근거

ORD 기록
ord-94c8912e57f04c18885594bb17ef660b
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07220695B2

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