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Hydrochloric Acid → 1-(Cyclopropylmethyl)-2-(4-ethoxybenzyl)-5-(1-pyrrolidinylcarbonyl)-1H-benzimidazole

HRID 1796479
ノート
印刷プレビュー

反応式

HRID 1796479 の反応式
[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([C:14](O)=[O:15])=[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=NC2[CH:38]=[CH:39][CH:40]=[N:41][C:36]1=2)=[N+](C)C)C.F[P-](F)(F)(F)(F)F.CCN(C(C)C)C(C)C.N1CCCC1.Cl>CN(C=O)C.C(OCC)C>[CH:1]1([CH2:4][N:5]2[C:9]3[CH:10]=[CH:11][C:12]([C:14]([N:41]4[CH2:40][CH2:39][CH2:38][CH2:36]4)=[O:15])=[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)[CH2:2][CH2:3]1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 313Hydrochloric AcidHCID 31268PyrrolidineHCID 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 22181275
1-(Cyclopropylmethyl)-2-(4-ethoxybenzyl)-5-(1-pyrrolidinylcarbonyl)-1H-benzimidazole
収率 89.1%

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

Following the general procedure 20E, 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 being stirred for 10 min, pyrrolidine (0.456 mmol) was added and the resulting mixture was stirred overnight. The crude residue after work-up 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 (82 mg, 79%). 1H N (400 MHz, CD3OD): δ 7.85 (s, 1H), 7.59 (d, J=8.6 Hz, 1H), 7.48 (d, J=8.6 Hz, 1H), 7.18 (d, J=8.1 Hz, 2H), 6.87 (d, J=8.1 Hz, 2H), 4.32 (s, 2H), 4.07 (d, J=6.8 Hz, 2H), 4.00 (q, J=7.6 Hz, 2H), 3.64 (t, J=. 7.2 Hz, 2H), 3.53 (t, J=7.2 Hz, 2H), 2.06–1.96 (m, 2H), 1.96–1.85 (m, 2H), 1.36 (t, J=7.6 Hz, 3H), 1.10–1.04 (m, 1H), 0.52–0.46 (m, 2H), 0.34–0.28 (m, 2H). MS (ESI) (M+H)+=404. Anal. Calcd for C25H29N3O2.1.5HCl: C, 65.53; H, 6.71; N, 9.17. Found: C, 65.48; H, 6.77; N, 8.75.

後処理

  1. stirringthe resulting mixture was stirred overnight
  2. customThe crude residue after work-up was purified by silica gel column chromatography
  3. customto give pure product which

出典と根拠

ORDレコード
ord-a546e29150934642a7b4067f7d32d648
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

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