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llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
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1-Ethyl-3-(3'-dimethylaminopropyl)carbodiimide → 14-cyclohexyl-6[2-(dimethylamino)ethyl]-N-(morpholin-4-ylsulfonyl)-5,6,7,8-tetrahydroindolo[2,1-a][2,5]benzodiazocine-11-carboxamide

HRID 1714077
ノート
印刷プレビュー

反応式

HRID 1714077 の反応式
[Cl-].[Cl-].[C:3]([C:6]1[CH:7]=[CH:8][C:9]2[C:10]([CH:30]3[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]3)=[C:11]3[C:18]4[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=4[CH2:16][NH+:15]([CH2:23][CH2:24][NH+:25]([CH3:27])[CH3:26])[CH2:14][CH2:13][N:12]3[C:28]=2[CH:29]=1)(O)=[O:4].[N:36]1([S:42]([NH2:45])(=[O:44])=[O:43])[CH2:41][CH2:40][O:39][CH2:38][CH2:37]1.CCN=C=NCCCN(C)C>CN(C1C=CN=CC=1)C>[CH:30]1([C:10]2[C:9]3[CH:8]=[CH:7][C:6]([C:3]([NH:45][S:42]([N:36]4[CH2:41][CH2:40][O:39][CH2:38][CH2:37]4)(=[O:44])=[O:43])=[O:4])=[CH:29][C:28]=3[N:12]3[CH2:13][CH2:14][N:15]([CH2:23][CH2:24][N:25]([CH3:26])[CH3:27])[CH2:16][C:17]4[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=4[C:11]=23)[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 2767394-MorpholinesulfonamideHCID 8660497211-Carboxy-14-cyclohexyl-6-[2-(dimethylammonio)ethyl]-5,6,7,8-tetrahydroindolo-[2,1-a][2,5]benzodiazocin-6-ium dichloride

生成物 1

HCID 6850842414-cyclohexyl-6[2-(dimethylamino)ethyl]-N-(morpholin-4-ylsulfonyl)-5,6,7,8-tetrahydroindolo[2,1-a][2,5]benzodiazocine-11-carboxamide収率 31%

試薬・触媒・溶媒 1

HCID 142844-(Dimethylamino)pyridine触媒

実験手順

To 11-carboxy-14-cyclohexyl-6-[2-(dimethylammonio)ethyl]-5,6,7,8-tetrahydroindolo-[2,1-a][2,5]benzodiazocin-6-ium dichloride (1 eq) (prepared from the product described in Example 20, Step 5, by iterative freeze drying in the presence of aqueous HCl) in DCM (0.06 M) was added morpholine-4-sulfonamide (1.5 eq), EDCI (1.5 eq) and DMAP (1.5 eq). The solution was stirred at RT overnight. The solvent was evaporated in vacuo and the crude was purified by automated RP-MS-HPLC (stationary phase: column Waters SYMMETRY prep. C18, 7 μm, 19×300 mm. Mobile phase: MeCN/H2O buffered with 0.1 TFA). Fractions containing the pure compound were combined and freeze dried to afford the title compound as a white powder (31%).

後処理

  1. dry with materialdrying in the presence of aqueous HCl) in DCM (0.06 M)
  2. customThe solvent was evaporated in vacuo
  3. customthe crude was purified by automated RP-MS-HPLC (stationary phase: column Waters SYMMETRY prep. C18, 7 μm, 19×300 mm. Mobile phase: MeCN/H2O buffered with 0.1 TFA)
  4. additionFractions containing the pure compound
  5. customfreeze dried

出典と根拠

ORDレコード
ord-53260fd0e7004b4eae6e135876d9ef0e
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07795247B2

反応ノート

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