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Diisopropylethylamine → HCID 59384387, 화합물

HRID 2357074
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HRID 2357074 반응식
[C:1]([O:5][C:6]([N:8]1[C@@:12]([CH3:16])([C:13]([OH:15])=O)[CH2:11][O:10][C:9]1([CH3:18])[CH3:17])=[O:7])([CH3:4])([CH3:3])[CH3:2].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.[CH2:52]([S:60][C:61]1[CH:70]=[CH:69][C:64]([C:65]([NH:67][NH2:68])=[O:66])=[CH:63][C:62]=1[C:71]([F:74])([F:73])[F:72])[CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH3:59].C([O-])(O)=O.[Na+]>CN(C=O)C.C1COCC1>[CH3:17][C:9]1([CH3:18])[N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:3])[CH3:4])=[O:7])[C@@:12]([CH3:16])([C:13]([NH:68][NH:67][C:65](=[O:66])[C:64]2[CH:69]=[CH:70][C:61]([S:60][CH2:52][CH2:53][CH2:54][CH2:55][CH2:56][CH2:57][CH2:58][CH3:59])=[C:62]([C:71]([F:72])([F:73])[F:74])[CH:63]=2)=[O:15])[CH2:11][O:10]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 81531DiisopropylethylamineHCID 516892Sodium BicarbonateHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 52987736HCID 52987736, 화합물HCID 59384425HCID 59384425, 화합물

생성물 1

HCID 59384387
HCID 59384387, 화합물
수율 84%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of (R)-3-(tert-butoxycarbonyl)-2,2,4-trimethyloxazolidine-4-carboxylic acid 4 (129.6 mg, 0.5 mmol) in DMF (1 mL) was added HATU (209 mg, 0.55 mol) and DIPEA (0.436 mL, 2.5 mmol). After being stirred at rt for 10 min, the reaction mixture was treated with 4-(octylthio)-3-(trifluoromethyl)benzohydrazide 3a (174 mg, 0.5 mmol) in THF (2 mL) and was left stirred overnight. Aqueous NaHCO3 solution was added and the mixture was extracted with EtOAc. The organic layer was washed with brine, dried over anhydrous Na2SO4, and evaporated under reduced pressure to give a residue, which was purified by SiO2 column chromatograph (n-hexane/EtOAc=3:7) to give (R)-tert-butyl 2,2,4-trimethyl-4-(2-(4-(octylthio)-3-(trifluoromethyl)benzoyl)hydrazinecarbonyl)oxazolidine-3-carboxylate 5a (247 mg, 84%). HPLC retention time on a C18 column (30×4.6 mm, 3.5μ) was 3.08 min with gradient 10-95% acetonitrile-H2O (0.1% TFA) in 3.5 min as mobile phase. MS (ESI, M+H+)=590.5

후처리

  1. waitwas left
  2. stirringstirred overnight
  3. extractionthe mixture was extracted with EtOAc
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. customevaporated under reduced pressure
  7. customto give a residue, which
  8. customwas purified by SiO2 column chromatograph (n-hexane/EtOAc=3:7)

출처 및 근거

ORD 기록
ord-4fcc7fc2b2fc4397b9a35ce27e40cad7
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07759370B2

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