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Hydrochloric Acid → 2-(4-ethoxybenzyl)-N-cyclohexyl-1-(cyclopropylmethyl)-N-methyl-1H-benzo[d]imidazole-5-carboxamide

HRID 1796478
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HRID 1796478 반응식
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([C:14]([OH:16])=O)=[CH:13][C:8]=3[N:7]=[C:6]2[CH2:17][C:18]2[CH:23]=[CH:22][C:21]([O:24][CH2:25][CH3:26])=[CH:20][CH:19]=2)[CH2:3][CH2:2]1.CN(C(ON1N=N[C:37]2[CH:38]=[CH:39][CH:40]=[N:41][C:36]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.[CH3:51][CH2:52]N(C(C)C)C(C)C.C1(CN)CCCCC1.Cl>CN(C=O)C.CCOC(C)=O.C(OCC)C>[CH:40]1([N:41]([CH3:36])[C:14]([C:12]2[CH:11]=[CH:10][C:9]3[N:5]([CH2:4][CH:1]4[CH2:3][CH2:2]4)[C:6]([CH2:17][C:18]4[CH:19]=[CH:20][C:21]([O:24][CH2:25][CH3:26])=[CH:22][CH:23]=4)=[N:7][C:8]=3[CH:13]=2)=[O:16])[CH2:39][CH2:38][CH2:37][CH2:52][CH2:51]1
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참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 76688CyclohexanemethylamineHCID 81531DiisopropylethylamineHCID 9886157Methanaminium, N-((dimethylamino)(3H-1,2,3-triazolo(4,5-b)pyridin-3-yloxy)methylene)-N-methyl-, hexafluorophosphate(1-) (1:1)HCID 22181336HCID 22181336, 화합물

생성물 1

HCID 22181387
2-(4-ethoxybenzyl)-N-cyclohexyl-1-(cyclopropylmethyl)-N-methyl-1H-benzo[d]imidazole-5-carboxamide
수율 91.5%

시약·촉매·용매 3

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

1-(Cyclopropylmethyl)-2-(4-ethoxybenzyl)-1H-benzimidazole-5-carboxylic acid (80 mg, 0.228 mmol) was dissolved in DMF (2 mL) and then HATU (104 mg, 0.274 mmol) was added followed by DIPEA (48 μL, 0.274 mmol). After stirring for 10 min; cyclohexylmethyl amine (0.456 mmol) was added and the resulting mixture was stirred overnight. The mixture was diluted with EtOAc (50 mL), washed with saturated NaHCO3 (2×10 mL) and then H2O (2×10 mL), dried over MgSO4, and concentrated to give a crude amide. The crude residue was purified by silica gel column chromatography to give pure product which was treated with 1 M HCl solution in diethyl ether to form a HCl salt as white solids (93 mg, 78%). 1H NMR (400 MHz, CD3OD): δ 7.66 (s, 1H), 7.58 (d, J=8.0 Hz, 1H), 7.30 (d, J=8.0 Hz, 1H), 7.16 (d, J=8.6 Hz, 2H), 6.84 (d, J=8.6 Hz, 2H), 4.30 (s, 2H), 4.10–4.04 (m, 5H), 3.96 (q, J=7.6 Hz, 2H), 3.66–3.54 (m, 1H), 1.90–1.50 (m, 10H), 1.33 (t, J=7.6 Hz, 3H), 1.10–0.98 (m, 1H), 0.50–0.42 (m, 2H), 0.32–0.27 (m, 2H). MS (ESI) (M+H)+=446. Anal. Calcd for C28H35N3O2.2.2HCl: C, 63.96; H, 7.13; N, 7.99. Found: C, 64.11; H, 7.24; N, 7.73.

후처리

  1. stirringthe resulting mixture was stirred overnight
  2. washwashed with saturated NaHCO3 (2×10 mL)
  3. dry with materialH2O (2×10 mL), dried over MgSO4
  4. concentrationconcentrated
  5. customto give a crude amide
  6. customThe crude residue was purified by silica gel column chromatography
  7. customto give pure product which

출처 및 근거

ORD 기록
ord-1862c08c0c88430ca007a43e1bec649c
출처 데이터셋
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07030139B2

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