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

HRID 1796478
ノート
印刷プレビュー

反応式

HRID 1796478 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 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、化合物

生成物 1

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

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-1862c08c0c88430ca007a43e1bec649c
出典データセット
uspto-grants-2006_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07030139B2

反応ノート

読み込み中…

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