Diisopropylethylamine → 5-Chloro-thiophene-2-carboxylic acid [(S)-2-(2-ethyl-3-pyridin-2-yl-benzene-sulfonylamino)-3-((S)-3-methyl-morpholin-4-yl)-3-oxo-propyl]-amide hydro chloride

HRID 389665ノート

反応式

HRID 389665 の反応式
[CH2:1]([C:3]1[C:8](N2CCOCC2=O)=[CH:7][CH:6]=[CH:5][C:4]=1[S:16]([NH:19][C@H:20]([C:31]([N:33]1[CH2:38][CH2:37][O:36][C@H:35](C)[CH2:34]1)=[O:32])[CH2:21][NH:22][C:23]([C:25]1[S:26][C:27]([Cl:30])=[CH:28][CH:29]=1)=[O:24])(=[O:18])=[O:17])[CH3:2].[CH3:40]CN(C(C)C)C(C)C.C(C1C([C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][N:58]=2)=CC=CC=1S(Cl)(=O)=O)C>C(Cl)Cl>[ClH:30].[CH2:1]([C:3]1[C:8]([C:57]2[CH:62]=[CH:61][CH:60]=[CH:59][N:58]=2)=[CH:7][CH:6]=[CH:5][C:4]=1[S:16]([NH:19][C@H:20]([C:31]([N:33]1[CH2:38][CH2:37][O:36][CH2:35][C@@H:34]1[CH3:40])=[O:32])[CH2:21][NH:22][C:23]([C:25]1[S:26][C:27]([Cl:30])=[CH:28][CH:29]=1)=[O:24])(=[O:17])=[O:18])[CH3:2]

参加物

5

反応物 3

HCID 81531DiisopropylethylamineHCID 442008575-Chloro-thiophene-2-carboxylic acid [(S)-2-[2-ethyl-3-(3-oxo-morpholin-4-yl)-benzenesulfonylamino]-3-((R)-2-methyl-morpholin-4-yl)-3-oxo-propyl]-amide2 回HCID 866532952-Ethyl-3-pyridin-2-yl-benzenesulfonyl chloride

生成物 1

HCID 671554425-Chloro-thiophene-2-carboxylic acid [(S)-2-(2-ethyl-3-pyridin-2-yl-benzene-sulfonylamino)-3-((S)-3-methyl-morpholin-4-yl)-3-oxo-propyl]-amide hydro chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

5-Chloro-thiophene-2-carboxylic acid [(S)-2-amino-3-((S)-3-methyl-morpholin-4-yl)-3-oxo-propyl]-amide (Intermediate 3) (95 mg, 0.287 mmol) was dissolved in 2 ml DCM and DIPEA (151 μl, 0.861 mmol). Intermediate 61 (81 mg, 0.287 mmol) in 2 ml DCM was slowly added and the reaction was stirred for 1.5 h. Then the solution was evaporated to dryness and purified by prep. HPLC. After lyophilization the title compound is obtained as colorless, amorphous solid. The material was dissolved in 20 ml water and 150 μl 4N HCl in dioxane were added. The solution was lyophilized again. Yield: 77 mg, 44%. MS (ES+): m/e=577.1/579.1, chloro pattern.

後処理

  1. customThen the solution was evaporated to dryness
  2. custompurified by prep

出典と根拠

ORDレコード
ord-0f4a870dd4704cdcb9e18c411f5976a5
出典データセット
uspto-grants-2013_02
特許番号
US08378092B2

反応ノート

読み込み中…