Hydrochloric Acid → 4-((2-Carbamoyl-phenyl)-{3-chloro-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoyl}-amino)-butyric acid

HRID 2268653노트

반응식

HRID 2268653 반응식
[OH-].[Na+].FC(F)(F)C(O)=O.C[O:11][C:12](=[O:45])[CH2:13][CH2:14][CH2:15][N:16]([C:36]1[CH:41]=[CH:40][CH:39]=[CH:38][C:37]=1[C:42](=[O:44])[NH2:43])[C:17](=[O:35])[C:18]1[CH:23]=[C:22]([O:24][CH2:25][CH2:26][NH:27][C:28]2[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=2)[CH:21]=[C:20]([Cl:34])[CH:19]=1.Cl>O1CCOCC1>[C:42]([C:37]1[CH:38]=[CH:39][CH:40]=[CH:41][C:36]=1[N:16]([C:17](=[O:35])[C:18]1[CH:23]=[C:22]([O:24][CH2:25][CH2:26][NH:27][C:28]2[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=2)[CH:21]=[C:20]([Cl:34])[CH:19]=1)[CH2:15][CH2:14][CH2:13][C:12]([OH:45])=[O:11])(=[O:44])[NH2:43]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 699502544-((2-Carbamoyl-phenyl)-{3-chloro-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoyl}-amino)-butyric acid methyl ester trifluoroacetate

생성물 1

HCID 183491504-((2-Carbamoyl-phenyl)-{3-chloro-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoyl}-amino)-butyric acid수율 100.6%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

2M Aqueous sodium hydroxide (0.200 ml) was added to a stirred solution of 4-((2-carbamoyl-phenyl)-{3-chloro-5-[2-(pyridin-4-ylamino)-ethoxy]-benzoyl}-amino)-butyric acid methyl ester trifluoroacetate (0.030 g) in 1,4-dioxan (1 ml). 2M Aqueous hydrochloric acid (0.2 ml) was added after 16 h. The reaction mixture was evaporated in vacuo and the residue was subjected to preparative hplc to give the title compound (0.024 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 reaction mixture was evaporated in vacuo

출처 및 근거

ORD 기록
ord-840eac500fe3486089edf5c49b7e398e
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06326386B1

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