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Water → N-(2-Carbamoyl-ethyl)-3-chloro-N-cyclobutyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

HRID 2268685
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인쇄 미리보기

반응식

HRID 2268685 반응식
C(OC(=O)[N:7]([CH2:14][CH2:15][O:16][C:17]1[CH:22]=[C:21]([C:23](=[O:33])[N:24]([CH2:29][CH2:30][C:31]#[N:32])[CH:25]2[CH2:28][CH2:27][CH2:26]2)[CH:20]=[C:19]([Cl:34])[CH:18]=1)[C:8]1[CH:13]=[CH:12][N:11]=[CH:10][CH:9]=1)(C)(C)C.[OH2:36].[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40]>ClCCl>[F:37][C:38]([F:43])([F:42])[C:39]([OH:41])=[O:40].[C:31]([CH2:30][CH2:29][N:24]([CH:25]1[CH2:28][CH2:27][CH2:26]1)[C:23](=[O:33])[C:21]1[CH:22]=[C:17]([O:16][CH2:15][CH2:14][NH:7][C:8]2[CH:9]=[CH:10][N:11]=[CH:12][CH:13]=2)[CH:18]=[C:19]([Cl:34])[CH:20]=1)(=[O:36])[NH2:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 6422Trifluoroacetic acidHCID 54411432(2-{3-Chloro-5-[(2-cyano-ethyl)-cyclobutyl-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tert-butyl ester

생성물 1

HCID 18349117N-(2-Carbamoyl-ethyl)-3-chloro-N-cyclobutyl-5-[2-(pyridin-4-ylamino)-ethoxy]-benzamide trifluoroacetate

시약·촉매·용매 1

HCID 6344Dichloromethane
용매

실험 절차

A solution of (2-{3-chloro-5-[(2-cyano-ethyl)-cyclobutyl-carbamoyl]-phenoxy}-ethyl)-pyridin-4-yl-carbamic acid tert-butyl ester (0.042 g) and water (0.050 ml) in mixture of trifluoroacetic acid (1 ml) and dichloromethane (1 ml) was stored at room temperature for 24 h and then the solvent removed under reduced pressure. The residue was subjected to preparative hplc to give the title compound (0.027 g) as a colourless gum by concentration of the required fraction under reduced pressure and drying by repetitive addition of acetonitrile and concentration under reduced pressure.

후처리

  1. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-534ea23a888a4bc0945f56d83c6621a5
출처 데이터셋
uspto-grants-2001_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06326386B1

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