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1,2-Dichloroethane → HCID 68703969, 화합물

HRID 1619223
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HRID 1619223 반응식
C(O[C:6]([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][N:11]([C:16]1[N:21]=[CH:20][CH:19]=[CH:18][N:17]=1)[CH2:12]2)=[O:7])(C)(C)C.FC(F)(F)C1[CH:25]=[C:26]([C:30]2[CH:35]=[CH:34][C:33](C(O)=O)=[CH:32][CH:31]=2)[CH:27]=CC=1.[CH2:41](Cl)[CH2:42]Cl.[CH:45]1[CH:46]=CC2N(O)N=N[C:49]=2[CH:50]=1.Cl.O1CCOC[CH2:57]1>O.CCOC(C)=O>[C:26]([C:30]1[CH:31]=[C:32]([C:42]2[CH:41]=[CH:49][C:50]([C:6]([N:8]3[CH:9]4[CH2:15][CH2:14][CH:13]3[CH2:12][N:11]([C:16]3[N:17]=[CH:18][CH:19]=[CH:20][N:21]=3)[CH2:10]4)=[O:7])=[CH:45][CH:46]=2)[CH:33]=[CH:34][CH:35]=1)([CH3:25])([CH3:27])[CH3:57]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 5

HCID 111,2-DichloroethaneHCID 757711-HydroxybenzotriazoleHCID 27827173'-(Trifluoromethyl)[1,1'-biphenyl]-4-carboxylic acidHCID 204431481,4-Dioxane hydrochlorideHCID 68700570HCID 68700570, 화합물

생성물 1

HCID 68703969HCID 68703969, 화합물수율 32%

시약·촉매·용매 2

HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

A solution of 3-pyrimidin-2-yl-3,8-diaza-bicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (64 mg, 0.22 mmol) in HCl/dioxane was stirred for 5 hours at room temperature. The resulting solution was concentrated, and the residue was dissolved in CH2Cl2 (5 mL) and added to a solution of 3′-trifluoromethyl-biphenyl-4-carboxylic acid (117 mg, 0.44 mmol), EDC (85 mg, 0.44 mmol), HOBt (60 mg, 0.44 mol) and TEA (0.1 mL, 0.71 mmol). After stirring overnight, the mixture was treated with EtOAc (50 mL) and water (15 mL). The organic phase was washed with brine (5 mL), dried (MgSO4), filtered, and concentrated under reduced pressure to furnish the crude product. This material was purified by column chromatography (30% EtOAc/hexanes) to give the title compound 14.2 mg, (32%) as a white solid: 1H NMR (DMSO): δ 8.35 (d, J=12 Hz, 2H), 7.79-7.76 (m, 3H), 7.68 (dt, J=20, 3 Hz, 1H), 7.63 (d, J=21 Hz, 2H), 7.52-7.43 (m, 2H), 6.62 (t, J=12 Hz, 1H), 4.77 (bs, 1H), 4.41 (d, J=64 Hz, 2H), 4.17 (bs, 1H), 3.14 (bs, 2H), 2.48 (qt, J=5 Hz, 1H), 1.86 (t, J=9 Hz, 2H), 1.60 (d, J=24 Hz, 1H); MS (M+1)=439.

후처리

  1. concentrationThe resulting solution was concentrated
  2. dissolutionthe residue was dissolved in CH2Cl2 (5 mL)
  3. washThe organic phase was washed with brine (5 mL)
  4. dry with materialdried (MgSO4)
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customto furnish the crude product
  8. customThis material was purified by column chromatography (30% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-a90f22ee11f645bab735ec4b6c5d2cd0
출처 데이터셋
uspto-grants-2014_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08772291B2

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