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Sodium Iodide → HCID 131736375, 화합물

HRID 1055481
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HRID 1055481 반응식
[CH3:1][N:2]([C@@H:10]([CH3:31])[C:11](=[O:30])[NH:12][CH:13]1[C:19]2([CH2:24][CH2:23][O:22][CH2:21][CH2:20]2)[O:18][C:17]2[CH:25]=[CH:26][CH:27]=[CH:28][C:16]=2[NH:15][C:14]1=[O:29])[C:3](=[O:9])[O:4][C:5]([CH3:8])([CH3:7])[CH3:6].Br[CH2:33][C:34]1[C:38]2[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=2[O:36][N:35]=1.C([O-])([O-])=O.[Cs+].[Cs+].[Na+].[I-]>CN(C=O)C.CCOC(C)=O>[O:36]1[C:37]2[CH:42]=[CH:41][CH:40]=[CH:39][C:38]=2[C:34]([CH2:33][N:15]2[C:14](=[O:29])[C@@H:13]([NH:12][C:11](=[O:30])[C@@H:10]([N:2]([CH3:1])[C:3](=[O:9])[O:4][C:5]([CH3:8])([CH3:6])[CH3:7])[CH3:31])[C:19]3([CH2:20][CH2:21][O:22][CH2:23][CH2:24]3)[O:18][C:17]3[CH:25]=[CH:26][CH:27]=[CH:28][C:16]2=3)=[N:35]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 10796Cesium carbonateHCID 34991891,2-Benzisoxazole, 3-(bromomethyl)-HCID 118574082HCID 118574082, 화합물

생성물 1

HCID 131736375HCID 131736375, 화합물수율 27%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 8857Ethyl Acetate용매

실험 절차

A mixture of tert-butyl methyl((2S)-1-oxo-1-(4-oxo-2′,3′,4,5,5′,6′-hexahydro-3H-spiro[benzo[b][1,4]oxazepine-2,4′-pyran]-3-ylamino)propan-2-yl)carbamate (156 mg, 360 μmol), 3-(bromomethyl)benzo[d]isoxazole (83.9 mg, 396 μmol), Cs2CO3 (141 mg, 432 μmol) and NaI (64.7 mg, 432 μmol) in DMF (900 μL) was stirred at RT for 18 h, diluted with EtOAc, washed with H2O, brine, dried over Na2SO4, filtered, and the filtrate concentrated to give a residue that was purified by silica gel chromatography. The resulting material was purified by supercritical fluid chromatography (SFC) to provide tert-butyl (S)-1-((S)-5-(benzo[d]isoxazol-3-ylmethyl)-4-oxo-2′,3′,4,5,5′,6′-hexahydro-3H-spiro[benzo[b][1,4]oxazepine-2,4′-pyran]-3-ylamino)-1-oxopropan-2-yl(methyl)carbamate (54.5 mg, 27%) as a white foam.

후처리

  1. washwashed with H2O, brine
  2. dry with materialdried over Na2SO4
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated
  5. customto give a residue that
  6. customwas purified by silica gel chromatography
  7. customThe resulting material was purified by supercritical fluid chromatography (SFC)

출처 및 근거

ORD 기록
ord-4e5754faa0d645ff98b8dc97985c1645
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394263B2

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