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Hydrochloric Acid → HCID 178515380、化合物

HRID 1096912
ノート
印刷プレビュー

反応式

HRID 1096912 の反応式
[CH:1]1([C:4]2[N:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:7]3[CH:15]=[CH:16][C:17]([C:19](OC)=[O:20])=[CH:18][C:6]=3[N:5]=2)[CH2:3][CH2:2]1.[OH-].[Na+].Cl.Cl.[NH:27]1[C:31]([C:32]2[CH:33]=[C:34]3[C:44](=[CH:45][CH:46]=2)[O:43][C:37]2([CH2:42][CH2:41][NH:40][CH2:39][CH2:38]2)[CH2:36][C:35]3=[O:47])=[N:30][N:29]=[N:28]1.C(N(CC)CC)C.C1C=CC2N(O)N=NC=2C=1.CCN=C=NCCCN(C)C.Cl>C1COCC1.CO.O.CN(C=O)C>[CH:1]1([C:4]2[N:8]([C:9]3[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=3)[C:7]3[CH:15]=[CH:16][C:17]([C:19]([N:40]4[CH2:41][CH2:42][C:37]5([CH2:36][C:35](=[O:47])[C:34]6[C:44](=[CH:45][CH:46]=[C:32]([C:31]7[NH:27][N:28]=[N:29][N:30]=7)[CH:33]=6)[O:43]5)[CH2:38][CH2:39]4)=[O:20])=[CH:18][C:6]=3[N:5]=2)[CH2:3][CH2:2]1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

12

反応物 7

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 14798Sodium HydroxideHCID 757711-HydroxybenzotriazoleHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 66782575HCID 66782575、化合物HCID 178479612HCID 178479612、化合物

生成物 1

HCID 178515380HCID 178515380、化合物

試薬・触媒・溶媒 4

HCID 887Methanol溶媒HCID 962Water溶媒2 回HCID 6228Dimethylformamide溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
60 °C

実験手順

Methyl 2-cyclopropyl-1-phenyl-1H-benzimidazole-5-carboxylate (194 mg, 0.664 mmol) was dissolved in THF (6 mL) and MeOH (6 mL), and aqueous 5 N sodium hydroxide solution (0.66 mL, 3.30 mmol) was added to it and stirred at 60° C. for 2 hours. This was restored to room temperature, 5 N hydrochloric acid (0.66 mL, 3.30 mmol) was added thereto, the solvent was evaporated away under reduced pressure, and the residue was azeotroped with toluene. DMF (4 mL) and water (1 mL) were added to it, and 6-(tetrazol-5-yl)spiro[chroman-2,4′-piperidin]-4-one hydrochloride (256 mg, 0.797 mmol), triethylamine (0.14 mL, 0.996 mmol), HOBT (135 mg, 0.996 mmol) and WSC hydrochloride (191 mg, 0.996 mmol) were added thereto. The reaction liquid was stirred at 90° C. for 2 hours, restored to room temperature, and water was added thereto. The precipitated solid was taken out through filtration, and dried under reduced pressure to obtain the title compound as a white solid. 1H-NMR (400 MHz, DMSO-d6) δ: 8.42 (1H, d, J=2.2 Hz), 8.23 (1H, dd, J=8.8, 2.2 Hz), 7.69-7.59 (6H, m), 7.34 (1H, d, J=8.8 Hz), 7.23 (1H, dd, J=8.4, 1.6 Hz), 7.14 (1H, d, J=8.4 Hz), 4.50-3.29 (5H, m), 2.98 (2H, s), 2.06-1.77 (4H, m), 1.15-1.11 (2H, m), 1.04-1.00 (2H, m). MS [M+H]+=546.

後処理

  1. customThis was restored to room temperature
  2. customthe solvent was evaporated away under reduced pressure
  3. customthe residue was azeotroped with toluene
  4. additionwere added
  5. customThe reaction liquid
  6. stirringwas stirred at 90° C. for 2 hours
  7. customrestored to room temperature
  8. filtrationThe precipitated solid was taken out through filtration
  9. customdried under reduced pressure

出典と根拠

ORDレコード
ord-1fbf4ef97e74427981522cd036cbf70e
出典データセット
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08138197B2

反応ノート

読み込み中…

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