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Methylamine → HCID 11391445, 화합물

HRID 1837219
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HRID 1837219 반응식
[CH3:1][NH2:2].IC[CH2:5][CH2:6][CH:7]([S:17][CH:18](CCCI)[CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23])CCC(F)(F)C(F)(F)F>O1CCCC1>[CH3:1][NH:2][CH2:5][CH2:6][CH2:7][S:17][CH2:18][CH2:19][CH2:20][C:21]([F:27])([F:26])[C:22]([F:25])([F:24])[F:23]
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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

45 g of methylamine is condensed in a solution of 30.6 g of 3-iodopropyl-4,4,5,5,5-pentafluoro-pentylsulfide in 200 ml of absolute tetrahydrofuran at a bath temperature of −78° C., and it is stirred for 1.5 hours at room temperature as well as for 4 hours at 60° C. in a 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 come to room temperature, excess methylamine is evaporated, it is 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-pentafluoro-pentylthio)-propyl]-amine is obtained as an oil.

후처리

  1. temperatureto cool overnight to room temperature
  2. customto −78° C
  3. customto come to room temperature
  4. customexcess methylamine is evaporated
  5. additionit is diluted with ethyl acetate
  6. washwashed neutral
  7. customdried on sodium sulfate
  8. concentrationconcentrated by evaporation in a vacuum
  9. customchromatographed on silica gel with dichloromethane/methanol

출처 및 근거

ORD 기록
ord-3e853f8779bc418ab06249047782d7e3
출처 데이터셋
uspto-grants-2004_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06780855B2

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