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Methylamine → HCID 11391445, 화합물

HRID 361688
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HRID 361688 반응식
IC[CH2:3][CH2:4][CH:5]([S:15][CH:16](CCCI)[CH2:17][CH2:18][C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21])CCC(F)(F)C(F)(F)F.[CH3:30][NH2:31]>O1CCCC1>[CH3:30][NH:31][CH2:3][CH2:4][CH2:5][S:15][CH2:16][CH2:17][CH2:18][C:19]([F:25])([F:24])[C:20]([F:23])([F:22])[F:21]
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참가 물질

4

반응물 2

HCID 6329MethylamineHCID 865876413-Iodopropyl-4,4,5,5,5-pentafluoropentylsulfide

생성물 1

HCID 11391445HCID 11391445, 화합물수율 133.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
60 °C

실험 절차

In a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoropentylsulfide in 200 ml of absolute tetrahydrofuran, 45 g of methylamine is condensed at a bath temperature of -78° C., and it is stirred for 1.5 hours at room temperature and for 4 hours at 60° C. in the pressurized reactor. To open the reactor, it is allowed to cool overnight to room temperature and then to -78° C. Then, it is allowed to reach room temperature, excess methylamine is evaporated, diluted with ethyl acetate, washed neutral, dried on sodium sulfate, concentrated by evaporation in a vacuum and chromatographed on silica gel with dichloromethane/methanol. 15.7 g of N-methyl-[3-(4,4,5,5,5-pentafluoropentylthio)-propyl]-amine is obtained as an oil.

후처리

  1. customcondensed at a bath temperature of -78° C., and it
  2. temperatureto cool overnight to room temperature
  3. customto -78° C
  4. customto reach room temperature
  5. customexcess methylamine is evaporated
  6. additiondiluted with ethyl acetate
  7. washwashed neutral
  8. customdried on sodium sulfate
  9. concentrationconcentrated by evaporation in a vacuum
  10. customchromatographed on silica gel with dichloromethane/methanol

출처 및 근거

ORD 기록
ord-3294caca39cf40688d15bb6d8d4eb66c
출처 데이터셋
uspto-grants-1999_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05866560

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