Hydrochloric Acid → {3-(4-Chlorophenyl)-5-oxo-4-[(1E)-3,3,3-trifluoroprop-1-en-1-yl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetic acid

HRID 709140ノート

反応式

HRID 709140 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12](/[CH:13]=[CH:14]/[C:15]([F:18])([F:17])[F:16])[C:11](=[O:19])[N:10]([CH2:20][C:21]([O:23]C)=[O:22])[N:9]=2)=[CH:4][CH:3]=1.[OH-].[Li+].Cl>CO.O.CS(C)=O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[N:12](/[CH:13]=[CH:14]/[C:15]([F:17])([F:16])[F:18])[C:11](=[O:19])[N:10]([CH2:20][C:21]([OH:23])=[O:22])[N:9]=2)=[CH:4][CH:3]=1

参加物

7

反応物 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 59536880Methyl {3-(4-chlorophenyl)-5-oxo-4-[(1E)-3,3,3-trifluoroprop-1-en-1-yl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetate

生成物 1

HCID 59536906{3-(4-Chlorophenyl)-5-oxo-4-[(1E)-3,3,3-trifluoroprop-1-en-1-yl]-4,5-dihydro-1H-1,2,4-triazol-1-yl}acetic acid

試薬・触媒・溶媒 3

HCID 679Dimethyl Sulfoxide溶媒HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

260 mg (0.72 mmol) of the compound of Example 32A were dissolved in 5 ml of methanol, and 2.87 ml (2.87 mmol) of a 1 M solution of lithium hydroxide in water were added. The mixture was stirred at RT for 1 h, then acidified with 1 N hydrochloric acid and diluted with DMSO. This solution was then purified directly by preparative HLPC [Method 9]. This gave 215 mg (86% of theory) of the title compound.

後処理

  1. customThis solution was then purified directly by preparative HLPC [Method 9]

出典と根拠

ORDレコード
ord-69e9f6f0387e4273b46776c109a6e5f8
出典データセット
uspto-grants-2015_11
特許番号
US09180120B2

反応ノート

読み込み中…