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1,2-Dichloroethane → tert-Butyl ((S)-1-((R)-3,3-dimethyl-5-(((R)-1,2,3,4-tetrahydronaphthalen-1-yl)carbamoyl)-1,3-azasilolidin-1-yl)-3-(4-iodophenyl)-1-oxopropan-2-yl)carbamate

HRID 527749
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HRID 527749 반응식
[C:1]([O:5][C:6]([NH:8][C@@H:9]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([I:20])=[CH:16][CH:15]=1)[C:10]([OH:12])=O)=[O:7])([CH3:4])([CH3:3])[CH3:2].C(Cl)CCl.N1C2C(=NC=CC=2)N(O)N=1.Cl.[CH3:36][Si:37]1([CH3:55])[CH2:41][C@@H:40]([C:42]([NH:44][C@H:45]2[C:54]3[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=3)[CH2:48][CH2:47][CH2:46]2)=[O:43])[NH:39][CH2:38]1.CCN(C(C)C)C(C)C>CN(C=O)C.C(OCC)(=O)C.[Cl-].[Na+].O>[CH3:36][Si:37]1([CH3:55])[CH2:41][C@@H:40]([C:42](=[O:43])[NH:44][C@H:45]2[C:54]3[C:49](=[CH:50][CH:51]=[CH:52][CH:53]=3)[CH2:48][CH2:47][CH2:46]2)[N:39]([C:10](=[O:12])[C@@H:9]([NH:8][C:6](=[O:7])[O:5][C:1]([CH3:2])([CH3:3])[CH3:4])[CH2:13][C:14]2[CH:19]=[CH:18][C:17]([I:20])=[CH:16][CH:15]=2)[CH2:38]1
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참가 물질

9

반응물 5

HCID 111,2-DichloroethaneHCID 81531DiisopropylethylamineHCID 181649HOAtHCID 2755956(2S)-2-{[(tert-butoxy)carbonyl]amino}-3-(4-iodophenyl)propanoic acidHCID 131735602(R)-3,3-dimethyl-N-((R)-1,2,3,4-tetrahydronaphthalen-1-yl)-1,3-azasilolidine-5-carboxamide HCl

생성물 1

HCID 131735601
tert-Butyl ((S)-1-((R)-3,3-dimethyl-5-(((R)-1,2,3,4-tetrahydronaphthalen-1-yl)carbamoyl)-1,3-azasilolidin-1-yl)-3-(4-iodophenyl)-1-oxopropan-2-yl)carbamate
수율 88.8%

시약·촉매·용매 3

HCID 6228Dimethylformamide용매2회HCID 8857Ethyl Acetate용매HCID 57417360Sodium chloride; water용매

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온도
0 °C

실험 절차

To a solution of (S)-2-((tert-butoxycarbonyl)amino)-3-(4-iodophenyl)propanoic acid (0.77 g, 2.0 mmol) in DMF (4 mL) was added EDC (0.53 g, 2.8 mmol) at 0° C. The reaction mixture was stirred at 0° C. for 5 min, followed by addition of 3H-[1,2,3]-triazolo[4,5-b]pyridin-3-ol (0.22 g, 1.6 mmol) and a solution of (R)-3,3-dimethyl-N—((R)-1,2,3,4-tetrahydronaphthalen-1-yl)-1,3-azasilolidine-5-carboxamide HCl (0.53 g, 1.6 mmol) in DMF (3 mL) and DIEA (0.8 mL, 4.6 mmol). The resulting mixture was then stirred at rt for 1 h and diluted with ethyl acetate and brine. The organic layer was separated, washed with aq. NaHCO3 solution, dried over MgSO4 and concentrated in vacuo. The resulting oil was purified by flash chromatography (eluting with 20% EtOAc/DCM) to afford the title compound as a white solid (0.94 g, 87%). 1H NMR (CDCl3) δ 7.76-7.45 (m, 2H), 7.22-7.05 (m, 3.5H), 6.89 (d, J=8.1 Hz, 2H), 6.50 (d, J=8.1 Hz, 0.5H), 5.27-5.06 (m, 3H), 4.96-4.71 (m, 1H), 3.10 (d, J=13.4 Hz, 0.5H), 2.96-2.45 (m, 4.5H), 2.16-1.98 (m, 1H), 1.85 (dd, J=11.3, 5.8 Hz, 3H), 1.44-1.16 (m, 10H), 0.98 (dd, J=14.7, 10.1 Hz, 1H), 0.44 (s, 3H), 0.27 (s, 3H); MS(ESI+) m/z 662.4 (M+H)+.

후처리

  1. stirringThe resulting mixture was then stirred at rt for 1 h
  2. customThe organic layer was separated
  3. washwashed with aq. NaHCO3 solution
  4. dry with materialdried over MgSO4
  5. concentrationconcentrated in vacuo
  6. customThe resulting oil was purified by flash chromatography (eluting with 20% EtOAc/DCM)

출처 및 근거

ORD 기록
ord-02d3bc875be34697bf9e063e209d6bd7
출처 데이터셋
uspto-grants-2016_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09345740B2

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