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Diisopropylethylamine → HCID 57971724, 화합물

HRID 2276987
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HRID 2276987 반응식
[CH2:1]([O:5][CH:6]([O:8][NH:9][C:10]([CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]([OH:20])=O)=[O:11])[CH3:7])[CH:2]([CH3:4])[CH3:3].C[Si](C)(C)[O:23][CH2:24][C:25]1[CH:30]=[CH:29][C:28]([NH2:31])=[CH:27][CH:26]=1.C1CN([P+](Br)(N2CCCC2)N2CCCC2)CC1.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C>CN(C=O)C.O.C(OCC)(=O)C>[CH2:1]([O:5][CH:6]([O:8][NH:9][C:10](=[O:11])[CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][C:18]([NH:31][C:28]1[CH:29]=[CH:30][C:25]([CH2:24][OH:23])=[CH:26][CH:27]=1)=[O:20])[CH3:7])[CH:2]([CH3:3])[CH3:4]
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참가 물질

8

반응물 4

HCID 81531DiisopropylethylamineHCID 2733179PyBroPHCID 11401321403613-26-3HCID 57971679HCID 57971679, 화합물

생성물 1

HCID 57971724HCID 57971724, 화합물수율 529.1%

시약·촉매·용매 3

HCID 962Water용매
HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

7-(1-Isobutoxy-ethoxycarbamoyl)-heptanoic acid (5.0 g, 1.72 mmol, 1.0 eq) and 4-trimethylsilanyloxymethyl-phenylamine (3.38 g, 1.72 mmol, 1.0 eq) were stirred together in DMF (140 mL). To the mixture was added PyBroP (10.5 g, 2.25 mmol, 1.3 eq) and DiPEA (3.9 mL, 2.25 mmol, 1.3 eq). The reaction was stirred under a nitrogen atmosphere overnight at room temperature. Ethyl acetate (200 mL) and water (200 mL) were added. The aqueous phase was isolated and re-extracted with ethyl acetate (2×100 mL). The combined organic phases were washed with water (2×50 mL) and brine (50 mL), then dried (MgSO4), filtered and concentrated in vacuo. The crude product was dissolved in the minimum of ethyl acetate and purified by passing through a pad of silica. The product was washed through the silica using ethyl acetate and collected in 100 mL conical flasks until elution ceased by LCMS analysis. Purification gave a yellow oil (3.59 g, 53% yield). LCMS purity 61%, m/z 417 [M++Na]+

후처리

  1. customThe aqueous phase was isolated
  2. extractionre-extracted with ethyl acetate (2×100 mL)
  3. washThe combined organic phases were washed with water (2×50 mL) and brine (50 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. dissolutionThe crude product was dissolved in the minimum of ethyl acetate
  8. custompurified
  9. washThe product was washed through the silica
  10. customcollected in 100 mL conical flasks until elution
  11. customPurification

출처 및 근거

ORD 기록
ord-af968a61ead54a239a9d58e766d0e7d4
출처 데이터셋
uspto-grants-2015_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09133104B2

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