Hydrochloric Acid → HCID 18542693、化合物

HRID 1268161ノート

反応式

HRID 1268161 の反応式
[ClH:1].Cl.Cl.[CH2:4]([N:11]([CH2:25]/[CH:26]=[CH:27]/[C:28]1[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=1)[C:31]([NH2:33])=[NH:32])[C:12]1[CH:17]=[CH:16][C:15]([O:18][CH:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)=[CH:14][CH:13]=1)[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.Cl.[C:38](=[NH:43])(OCC)[CH3:39].C(N(CC)CC)C.Cl>CO.O1CCOCC1>[ClH:1].[ClH:1].[ClH:1].[C:38]([N:22]1[CH2:21][CH2:20][CH:19]([O:18][C:15]2[CH:14]=[CH:13][C:12]([N:11]([CH2:25]/[CH:26]=[CH:27]/[C:28]3[CH:29]=[C:30]([CH:34]=[CH:35][CH:36]=3)[C:31]([NH2:33])=[NH:32])[CH2:4][C:5]3[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=3)=[CH:17][CH:16]=2)[CH2:24][CH2:23]1)(=[NH:43])[CH3:39]

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 8471TriethylamineHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 18542575HCID 18542575、化合物

生成物 1

HCID 18542693HCID 18542693、化合物収率 210%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒2 回HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 3-[3-[N-benzyl-N-[4-(piperidin-4-yloxy)phenyl]amino]-1-(E)-propenyl]benzamidine trihydrochloride (335 mg) in methanol (20 ml) were added ethyl acetimidate hydrochloride (230 mg) and triethylamine (0.51 ml) at room temperature. The resulting mixture was stirred at room temperature for 12 hours. To the reaction mixture was added a 4M solution of hydrogen chloride in dioxane (1 ml) and the solution was concentrated in vacuo. The residue was purified by preparative HPLC (YMC-Pack ODS YMC) using 30% aqueous acetonitrile as an eluant to afford an amorphous solid. To a solution of the solid in methanol (10 ml) was added a 4M solution of hydrogen chloride in dioxane (0.5 ml) and the mixture was concentrated to dryness in vacuo. A solution of the residual solid in water (about 10 ml) was lyophilized to give the title compound (252 mg, yield 70%) as a colorless amorphous solid.

後処理

  1. concentrationthe solution was concentrated in vacuo
  2. customThe residue was purified by preparative HPLC (YMC-Pack ODS YMC)
  3. customto afford an amorphous solid
  4. concentrationthe mixture was concentrated to dryness in vacuo

出典と根拠

ORDレコード
ord-8f61814b598d4bc2b8b1bcaf99aad399
出典データセット
uspto-grants-2003_04
特許番号
US06555556B1

反応ノート

読み込み中…