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Sodium Carbonate → (S)-2-amino-N-cyclopropyl-7'-(neopentyloxy)-5H-spiro[oxazole-4,9'-xanthene]-2'-carboxamide

HRID 1970347
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HRID 1970347 반응식
Br[C:2]1[CH:15]=[CH:14][C:13]2[O:12][C:11]3[C:6](=[CH:7][C:8]([O:16][CH2:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[CH:9][CH:10]=3)[C@:5]3([CH2:25][O:24][C:23]([NH2:26])=[N:22]3)[C:4]=2[CH:3]=1.[C:27](=[O:30])([O-])[O-].[Na+].[Na+].[CH:33]1([NH2:36])[CH2:35][CH2:34]1.O1CCOCC1>CCOC(C)=O.O.C(O[Pd]CC1C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C)(=O)C>[NH2:26][C:23]1[O:24][CH2:25][C@:5]2([N:22]=1)[C:4]1[CH:3]=[C:2]([C:27]([NH:36][CH:33]3[CH2:35][CH2:34]3)=[O:30])[CH:15]=[CH:14][C:13]=1[O:12][C:11]1[C:6]2=[CH:7][C:8]([O:16][CH2:17][C:18]([CH3:20])([CH3:19])[CH3:21])=[CH:9][CH:10]=1
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참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 312751,4-DioxaneHCID 69828CyclopropylamineHCID 58466128(R)-2'-bromo-7'-(neopentyloxy)-5H-spiro[oxazole-4,9'-xanthen]-2-amine

생성물 1

HCID 58466226(S)-2-amino-N-cyclopropyl-7'-(neopentyloxy)-5H-spiro[oxazole-4,9'-xanthene]-2'-carboxamide

시약·촉매·용매 3

HCID 178476741
HCID 178476741, 화합물
촉매
HCID 962Water용매
HCID 8857Ethyl Acetate용매

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온도
170 °C

실험 절차

A 0.5-2 mL microwave vial charged with (R)-2′-bromo-7′-(neopentyloxy)-5H-spiro[oxazole-4,9′-xanthen]-2-amine (0.1000 g, 0.240 mmol), Mo(CO)6 (0.063 g, 0.240 mmol), acetoxy(2-(dio-tolylphosphino)benzyl)palladium (0.011 g, 0.012 mmol), sodium carbonate (0.025 g, 0.240 mmol), cyclopropylamine (0.025 mL, 0.359 mmol), and 1,4-dioxane (0.443 mL, 5.03 mmol) was sealed and heated to 170° C. for 30 minutes. The mixture was diluted with EtOAc and water and filtered through celite. The celite was washed with EtOAc and MeOH. The aqueous phase was extracted with EtOAc three times. The organic layer was dried over Na2SO4 and concentrated in vacuo. The crude was purified by silica gel chromatography (2-10% MeOH—CH2Cl2, then 10% MeOH—CH2Cl2). The product was purified again by reverse phase prep HPLC: 10-55% CH3CN (0.1% TFA)-water (0.1% TFA) in 26 min. The fractions were combined and neutralized with solid Na2CO3, extracted three times with DCM. The organic layer was concentrated to provide (S)-2-amino-N-cyclopropyl-7′-(neopentyloxy)-5H-spiro[oxazole-4,9′-xanthene]-2′-carboxamide.

후처리

  1. customwas sealed
  2. filtrationfiltered through celite
  3. washThe celite was washed with EtOAc and MeOH
  4. extractionThe aqueous phase was extracted with EtOAc three times
  5. dry with materialThe organic layer was dried over Na2SO4
  6. concentrationconcentrated in vacuo
  7. customThe crude was purified by silica gel chromatography (2-10% MeOH—CH2Cl2
  8. customThe product was purified again by reverse phase prep HPLC
  9. extractionextracted three times with DCM
  10. concentrationThe organic layer was concentrated

출처 및 근거

ORD 기록
ord-60b6c5f58bbc48e6b5e3257634acf136
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08426447B2

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