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Hydrochloric Acid → HCID 78324790, 화합물

HRID 2201919
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HRID 2201919 반응식
[CH3:1][C@@H:2]1[CH2:6][CH2:5][CH2:4][N:3]1[CH2:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][C:18]([CH2:21][CH2:22][C:23](O)=[O:24])=[CH:17][CH:16]=2)=[CH:11][CH:10]=1.Cl.[NH2:27][C:28]([CH3:37])([CH3:36])[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30].CN(C(ON1N=NC2C=CC=NC1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.Cl>O1CCCC1.C(#N)C>[CH3:36][C:28]([NH:27][C:23](=[O:24])[CH2:22][CH2:21][C:18]1[CH:17]=[CH:16][C:15]([C:12]2[CH:13]=[CH:14][C:9]([CH2:8][CH2:7][N:3]3[CH2:4][CH2:5][CH2:6][C@H:2]3[CH3:1])=[CH:10][CH:11]=2)=[CH:20][CH:19]=1)([CH3:37])[C:29]([O:31][C:32]([CH3:35])([CH3:34])[CH3:33])=[O:30]
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 12186776Tert-butyl 2-amino-2-methylpropanoate hydrochlorideHCID 76286162HCID 76286162, 화합물

생성물 1

HCID 78324790HCID 78324790, 화합물

시약·촉매·용매 2

HCID 6342Acetonitrile용매
HCID 8028Tetrahydrofuran용매

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온도
60 °C

실험 절차

To a solution of (R)-3-(4′-(2-(2-methylpyrrolidin-1-yl)ethyl)biphenyl-4-yl)propanoic acid (40 mg, 0.119 mmol), tert-butyl 2-amino-2-methylpropanoate hydrochloride (27.8 mg, 0.142 mmol), and TEA (0.050 mL, 0.356 mmol) in tetrahydrofuran (1 mL) and acetonitrile (1 mL) was added HATU (54.1 mg, 0.142 mmol). The reaction mixture was stirred at 60° C. for 1.5 h and 1M HCl was added to neutralize the reaction solution. The resulting mixture was purified by HPLC to give the title compound. LCMS m/z=479.4 [M+H]+; 1H NMR (400 MHz, CD3CN) δ ppm 1.27 (d, J=6.9 Hz, 0.4H), 1.37 (s, 6H), 1.41 (s, 9H), 1.46 (d, J=6.5 Hz, 2.6H), 1.70-1.82 (m, 1H), 2.01-2.12 (m, 2H), 2.23-2.33 (m, 1H), 2.45 (t, J=7.8 Hz, 2H), 2.93 (t, J=7.6 Hz, 2H), 3.05-3.22 (m, 4H), 3.39-3.48 (m, 1H), 3.53-3.62 (m, 1H), 3.72-3.82 (m, 1H), 6.60 (s, 1H), 7.34 (d, J=8.2 Hz, 2H), 7.39 (d, J=8.2 Hz, 2H), 7.58 (d, J=8.2 Hz, 2H), 7.63 (d, J=8.2 Hz, 2H).

후처리

  1. customThe resulting mixture was purified by HPLC

출처 및 근거

ORD 기록
ord-de8bb1a70ef445b19d12e512d4686a95
출처 데이터셋
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09365511B2

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