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Sodium Bicarbonate → HCID 58179870, 화합물

HRID 1518561
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HRID 1518561 반응식
FC(F)(F)S(O[C:7]1[CH2:8][CH:9]2[N:14]([C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])[CH:12]([CH:13]=1)[CH2:11][CH2:10]2)(=O)=O.C([O-])(O)=O.[Na+].[F:29][C:30]1[C:35]([F:36])=[CH:34][CH:33]=[CH:32][C:31]=1[N:37]1[C:41]([C:42]2[C:43]([NH2:57])=[N:44][CH:45]=[C:46](B3OC(C)(C)C(C)(C)O3)[CH:47]=2)=[N:40][N:39]=[N:38]1>COCCOC.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[NH2:57][C:43]1[N:44]=[CH:45][C:46]([C:7]2[CH2:8][CH:9]3[N:14]([C:15]([O:17][C:18]([CH3:19])([CH3:20])[CH3:21])=[O:16])[CH:12]([CH:13]=2)[CH2:11][CH2:10]3)=[CH:47][C:42]=1[C:41]1[N:37]([C:31]2[CH:32]=[CH:33][CH:34]=[C:35]([F:36])[C:30]=2[F:29])[N:38]=[N:39][N:40]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 516892Sodium BicarbonateHCID 226480948-Boc-3-(trifluoromethylsulfonyloxy)-8-azabicyclo[3.2.1]oct-3-eneHCID 581794573-(1-(2,3-difluorophenyl)-1H-tetrazol-5-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-amine

생성물 1

HCID 58179870HCID 58179870, 화합물수율 51%

시약·촉매·용매 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 80711,2-Dimethoxyethane용매

실험 절차

A solution of tert-butyl 3-(trifluoromethylsulfonyloxy)-8-azabicyclo[3.2.1]oct-3-ene-8-carboxylate (50 mg, 140 μmol, 1.0 eq.) in DME (2 mL) was degassed with nitrogen for 15 minutes. NaHCO3 (1.2 mM solution, 350 μL, 420 μmol, 3 eq.) and 3-(1-(2,3-difluorophenyl)-1H-tetrazol-5-yl)-5-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridin-2-amine (56 mg, 140 μmol, 1.0 eq.) were added and degassing was continued for an additional 30 minutes. PdCl2(dppf)2 (10 mg, 14 μmol, 0.1 eq.) was added and degassing was continued for an additional 15 minutes. The reaction was sealed and microwaved at 90° C. for 15 minutes. After cooling, the organic layer was concentrated, NaHCO3 was added, and the product was extracted with EtOAc. Silica gel chromatography (EtOAc/hexanes) provided tert-butyl 3-(6-amino-5-(1-(2,3-difluorophenyl)-1H-tetrazol-5-yl)pyridin-3-yl)-8-azabicyclo[3.2.1]oct-3-ene-8-carboxylate (34 mg, 51% yield); 1H NMR (300 MHz, CDCl3): 8.25 (m, 1H); 7.6-7.25 (m, 3H); 7.07 (s, 1H); 6.4 (br s, 2H); 6.0 (m, 1H); 4.38 (m, 2H); 2.65 (m, 1H); 2.15 (m, 1H); 2.14-1.5 (m, 4H); 1.44 (s, 9H).

후처리

  1. customdegassing
  2. customdegassing
  3. waitwas continued for an additional 15 minutes
  4. customThe reaction was sealed
  5. custommicrowaved at 90° C. for 15 minutes
  6. temperatureAfter cooling
  7. concentrationthe organic layer was concentrated
  8. additionNaHCO3 was added
  9. extractionthe product was extracted with EtOAc

출처 및 근거

ORD 기록
ord-2a409b3277de4287b4ce5848027e9268
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08232406B2

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