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Diisopropylethylamine → 2-[3-(4-cyanobenzyl)-3H-imidazol-1-yl]-N-(4-cyanobenzyl)-N-(1-phenylpiperidin-4-yl)acetamide hydrochloride

HRID 1068505
ノート
印刷プレビュー

反応式

HRID 1068505 の反応式
[C:1]([C:3]1[CH:22]=[CH:21][C:6]([CH2:7][NH:8][CH:9]2[CH2:14][CH2:13][N:12]([C:15]3[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=3)[CH2:11][CH2:10]2)=[CH:5][CH:4]=1)#[N:2].[C:23]([C:25]1[CH:40]=[CH:39][C:28]([CH2:29][N:30]2[C:34](CC([O-])=O)=[CH:33][N:32]=[CH:31]2)=[CH:27][CH:26]=1)#[N:24].[Li+].[OH2:42].ON1C2C=CC=[CH:52][C:47]=2N=N1.[ClH:53].CN(C)CCCN=C=NCC.C(N(CC)C(C)C)(C)C>>[ClH:53].[C:23]([C:25]1[CH:26]=[CH:27][C:28]([CH2:29][N:30]2[CH:34]=[CH:33][N:32]([CH2:47][C:52]([N:8]([CH2:7][C:6]3[CH:5]=[CH:4][C:3]([C:1]#[N:2])=[CH:22][CH:21]=3)[CH:9]3[CH2:10][CH2:11][N:12]([C:15]4[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=4)[CH2:13][CH2:14]3)=[O:42])[CH2:31]2)=[CH:39][CH:40]=1)#[N:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 5

HCID 81531DiisopropylethylamineHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 27960291-Hydroxybenzotriazole hydrateHCID 21193414HCID 21193414、化合物HCID 67586058HCID 67586058、化合物

生成物 1

HCID 21193223
2-[3-(4-cyanobenzyl)-3H-imidazol-1-yl]-N-(4-cyanobenzyl)-N-(1-phenylpiperidin-4-yl)acetamide hydrochloride

実験手順

4-Cyanobenzyl(1-phenylpiperidin-4-yl)amine (75 mg, 0.26 mmol), lithium [3-(4-cyanobenzyl)-3H-imidazol-4-yl]acetate (70 mg, 0.28 mmol), 1-hydroxybenzotriazole hydrate (52 mg, 0.38 mmol), 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (99 mg, 0.52 mmol), and N,N-diisopropylethylamine (67 μL, 0.38 mmol) were added to degassed DMF (3 mL) and the mixture was stirred for 18 hrs at room temperature then concentrated in vacuo. The residue was added to sat. NaHCO3(aq) (5 mL) and extracted with dichloromethane (3×3 mL). The combined organic extracts were dried over MgSO4, filtered, and concentrated under reduced pressure. The residue was chromatographed on silica gel, eluting with dichloromethane—2% methanol to give the product as a free base. This was lyophilized from HCl (aq)—acetonitrile to give the title compound as a white solid.

後処理

  1. customto degassed DMF (3 mL)
  2. concentrationthen concentrated in vacuo
  3. additionThe residue was added to sat. NaHCO3(aq) (5 mL)
  4. extractionextracted with dichloromethane (3×3 mL)
  5. dry with materialThe combined organic extracts were dried over MgSO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was chromatographed on silica gel
  9. washeluting with dichloromethane—2% methanol
  10. customto give the product as a free base

出典と根拠

ORDレコード
ord-836791aa023346fe8a3c580e4633ac28
出典データセット
uspto-grants-2001_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06248756B1

反応ノート

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