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

HRID 2268653ノート

反応式

HRID 2268653 の反応式
[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]

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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.

後処理

  1. customThe reaction mixture was evaporated in vacuo

出典と根拠

ORDレコード
ord-840eac500fe3486089edf5c49b7e398e
出典データセット
uspto-grants-2001_12
特許番号
US06326386B1

反応ノート

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