Triethylamine → HCID 44193376, 화합물

HRID 1855459노트

반응식

HRID 1855459 반응식
[N+]([O-])(O)=O.[N+]([O-])(O)=O.[CH3:9][O:10][C:11]1[CH:12]=[C:13]([NH:23][C:24]([NH2:26])=[NH:25])[CH:14]=[CH:15][C:16]=1[N:17]1[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18]1.CN(C)[CH:29]=[CH:30][C:31]([C:33]1[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=1)=O.C(N(CC)CC)C>C(O)C>[CH3:9][O:10][C:11]1[CH:12]=[C:13]([NH:23][C:24]2[N:26]=[C:31]([C:33]3[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=3)[CH:30]=[CH:29][N:25]=2)[CH:14]=[CH:15][C:16]=1[N:17]1[CH:21]=[C:20]([CH3:22])[N:19]=[CH:18]1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 3534603-(Dimethylamino)-1-phenyl-2-propen-1-oneHCID 178493228HCID 178493228, 화합물

생성물 1

HCID 44193376HCID 44193376, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of N-[3-methoxy-4-(4-methyl-imidazol-1-yl)-phenyl]-guanidine dinitrate (249 mg, 0.67 mmol), 3-(dimethylamino)-1-phenyl-2-propen-1-one (141 mg, 0.80 mmol, CAS 1131-80-2) and triethyl amine (187 uL. 1.34 mmol) in ethanol (4 mL) was heated to 160° C. for 1 hour in a microwave oven. The solvent was evaporated under reduced pressure and the residue purified by column chromatography on silica using methylenechloride and dichloromethane/methanol (19:1 v/v) as eluent to yield the title compound a a yellow solid (67 mg, 28%). MS ISP (m/e): 358.2 (100) [(M+H)+]. 1H NMR (DMSO-D6, 300 MHz): δ (ppm)=9.90 (s, 1H), 8.60 (s, 1H), 8.20 (br s, 2H), 7.99 (s, 1H), 7.68 (s, 1H), 7.43-7.56 (m, 5H), 7.26 (t, 1H), 7.06 (s, 1H), 3.84 (s, 3H), 2.15 (s, 3H).

후처리

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue purified by column chromatography on silica

출처 및 근거

ORD 기록
ord-99e2b4c1a08749c7bdd70bc8dd937074
출처 데이터셋
uspto-grants-2015_02
특허 번호
US08962834B2

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