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Triphenylphosphine Oxide → HCID 57476116, 화합물

HRID 1994738
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HRID 1994738 반응식
C1(P(=O)(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.FC(F)(F)S(OS(C(F)(F)F)(=O)=O)(=O)=O.C([S:43][C:44]([CH3:82])([CH2:59][NH:60][C:61]([C:63]1[NH:64][C:65]2[C:70]([CH:71]=1)=[CH:69][CH:68]=[CH:67][C:66]=2[N:72]([CH3:81])[S:73]([C:76]1[S:77][CH:78]=[CH:79][CH:80]=1)(=[O:75])=[O:74])=O)[CH2:45][N:46]1[CH2:51][CH2:50][N:49](C(OC(C)(C)C)=O)[CH2:48][CH2:47]1)C1C=CC=CC=1.C(=O)([O-])O.[Na+]>C(#N)C>[CH3:81][N:72]([C:66]1[CH:67]=[CH:68][CH:69]=[C:70]2[C:65]=1[NH:64][C:63]([C:61]1[S:43][C:44]([CH3:82])([CH2:45][N:46]3[CH2:51][CH2:50][NH:49][CH2:48][CH2:47]3)[CH2:59][N:60]=1)=[CH:71]2)[S:73]([C:76]1[S:77][CH:78]=[CH:79][CH:80]=1)(=[O:75])=[O:74]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 13097Triphenylphosphine OxideHCID 67749Trifluoromethanesulfonic anhydrideHCID 516892Sodium BicarbonateHCID 59135589HCID 59135589, 화합물

생성물 1

HCID 57476116HCID 57476116, 화합물수율 45.1%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

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온도
0 °C

실험 절차

To a solution of triphenylphosphine oxide (3.09 g) in acetonitrile (20 ml) was slowly added trifluoromethanesulfonic anhydride (0.93 ml) at 0° C., and the mixture was stirred for 10 min. tert-Butyl 4-{2-(benzylthio)-2-methyl-3-[({7-[methyl(2-thienylsulfonyl)amino]-1H-indol-2-yl}carbonyl)amino]propyl}piperazine-1-carboxylate (1.55 g) was added, and the reaction mixture was stirred at 0° C. for 30 min. Saturated aqueous sodium hydrogencarbonate was added, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, and dried (MgSO4). 4N Hydrogen chloride-ethyl acetate solution was added to the ethyl acetate layer, and the precipitated solid was collected by filtration, and washed with ethyl acetate. The obtained solid was suspended in saturated aqueous sodium hydrogencarbonate, and the mixture was stirred for 30 min. The solid was collected by filtration, washed with water and ethyl acetate, and dried to give the title compound (0.49 g, yield 45%) as colorless crystals. melting point 178-180° C.

후처리

  1. customat 0° C.
  2. additionwas added
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. addition4N Hydrogen chloride-ethyl acetate solution was added to the ethyl acetate layer
  7. filtrationthe precipitated solid was collected by filtration
  8. washwashed with ethyl acetate
  9. stirringthe mixture was stirred for 30 min
  10. filtrationThe solid was collected by filtration
  11. washwashed with water and ethyl acetate
  12. customdried

출처 및 근거

ORD 기록
ord-00f82daa47d84bcbbf4a199d8b8bdd8c
출처 데이터셋
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07652133B2

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