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 389665노트

반응식

HRID 389665 반응식
[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]

참가 물질

5

반응물 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]-amide2회HCID 866532952-Ethyl-3-pyridin-2-yl-benzenesulfonyl chloride

생성물 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

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-0f4a870dd4704cdcb9e18c411f5976a5
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08378092B2

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