Acetonitrile → HCID 10340730, 화합물

HRID 585997

반응식

HRID 585997 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([N:12]=[C:13]=[O:14])[CH:8]=[CH:7][CH:6]=2.[N:15]1([C:21]2[CH:28]=[CH:27][C:24]([CH2:25][NH2:26])=[CH:23][CH:22]=2)[CH2:20][CH2:19][O:18][CH2:17][CH2:16]1.C(N(CC)CC)C.CC#N>C(OCC)C>[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[C:10]([CH:11]=1)=[C:9]([NH:12][C:13]([NH:26][CH2:25][C:24]1[CH:23]=[CH:22][C:21]([N:15]3[CH2:20][CH2:19][O:18][CH2:17][CH2:16]3)=[CH:28][CH:27]=1)=[O:14])[CH:8]=[CH:7][CH:6]=2

참가 물질

6

반응물 4

HCID 6342AcetonitrileHCID 8471TriethylamineHCID 27764584-MorpholinobenzylamineHCID 22337685HCID 22337685, 화합물

생성물 1

HCID 10340730HCID 10340730, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매2회

실험 절차

The product from Example 176A in diethyl ether (40 mL) was treated with the product from Example 172B (300 mg, 1.56 mmol) and triethylamine (3 mL) in 1:1 diethyl ether:CH3CN (10 mL). After stirring for 3 hours, the mixture was filtered, and the collected solid was washed with diethyl ether. The solid was purified by silica gel chromatography (95:5 CH2Cl2:MeOH) to provide the title compound. 1H NMR (300 MHz, DMSO-d6) δ 9.18 (s, 1H), 8.71 (s, 1H), 8.37 (d, 1H, J=6.7 Hz), 8.08 (s, 1H), 7.79 (d, 2H, J=8.2 Hz), 7.63 (t, 1H, J=8.0 Hz), 7.23 (d, 2H, J=8.7 Hz), 6.94 (d, 2H, J=8.4 Hz), 6.91 (t, 1H, 5.5 Hz), 4.26 (d, 2H, 5.7 Hz), 3.73 (m, 4H), 3.07 (m, 4H); MS (ESI+) m/z 397/399 (M+H, 35Cl/37Cl).

후처리

  1. filtrationthe mixture was filtered
  2. washthe collected solid was washed with diethyl ether
  3. customThe solid was purified by silica gel chromatography (95:5 CH2Cl2:MeOH)

출처 및 근거

ORD 기록
ord-1db545bf6a3d4ed09a1499399ec085d5
출처 데이터셋
uspto-grants-2005_08
특허 번호
US06933311B2

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