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P,P-Diphenylphosphinic azide → HCID 46200788, 화합물

HRID 1966461
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HRID 1966461 반응식
[CH2:1]([NH:8][C:9]1[CH:17]=[C:16]([N:18]2[CH2:23][CH2:22][N:21]([C:24](=[O:31])[C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:20][CH2:19]2)[CH:15]=[CH:14]C=1C(O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:32]([OH:34])[CH3:33].N.C1(P([N:50]=[N+]=[N-])(C2C=CC=CC=2)=O)C=CC=CC=1>C1COCC1>[CH2:1]([NH:8][C:9]1[CH:17]=[C:16]([N:18]2[CH2:23][CH2:22][N:21]([C:24](=[O:31])[C:25]3[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=3)[CH2:20][CH2:19]2)[CH:15]=[CH:14][C:33]=1[C:32]([NH2:50])=[O:34])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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HCID 199401P,P-Diphenylphosphinic azideHCID 22020343Ethanol, reaction products with ammonia, distn. residuesHCID 584256602-(Benzylamino)-4-(4-benzoylpiperazin-1-yl)benzoic acid

생성물 1

HCID 46200788HCID 46200788, 화합물수율 48.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 2-(benzylamino)-4-(4-benzoylpiperazin-1-yl)benzoic acid (80 mg, 0.2 mmol), 2 M ammonia ethanol solution (0.60 ml, 1.2 mmol), tiethylamine (0.08 ml, 0.57 mmol) and diphenylphosphoryl azide (0.045 ml, 0.2 mmol) in 15 ml THF was stirred for 16 hours. The run was quenched with 1 ml water and all the solvents were evaporated under vacuum. 2-(benzylamino)-4-(4-bezoylpiperazin-1-yl)benzamide (40 mg, 40%) was obtained by flash column chromatograph (60% ethyl acetate in hexanes), and its hydrochloride was made by bubbling HCL gas in ether solution. 1H NMR (500 MHz, DMSO-d6) δ (ppm) 3.28-3.670 (br, 8H), 4.43 (s, 2H), 5.00 (s, 1H), 6.06 (s, 1H), 6.24 (d, J=8.2 Hz, 1H), 7.00 (s, 1H), 7.12-7.65 (m, 13H), 7.67 (d, J=8.8 Hz, 1H). 13C NMR (125 MHz, DMSO-d6): δ (ppm) 43.5, 46.0, 95.3, 102.7, 127.0, 127.3, 128.3, 128.4, 128.5, 128.6, 129.6, 132.4, 136.0, 139.3, 151.7, 154.2, 167.0, 168.9.

후처리

  1. customThe run was quenched with 1 ml water and all the solvents
  2. customwere evaporated under vacuum

출처 및 근거

ORD 기록
ord-9503ecd5c6b44a3eb6ce9a3e4225965e
출처 데이터셋
uspto-grants-2013_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08420640B2

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