Hydrochloric Acid → 2-(2-Isopropylthiopyrid-3-yloxy)-propionic acid methyl ester

HRID 55549

反応式

HRID 55549 の反応式
[CH3:1][O:2][C:3](=[O:7])[CH:4](Br)[CH3:5].[CH:8]([S:11][C:12]1[C:17]([OH:18])=[CH:16][CH:15]=[CH:14][N:13]=1)([CH3:10])[CH3:9].C(=O)([O-])[O-].[K+].[K+].Cl>CN(C)C=O.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:7])[CH:4]([O:18][C:17]1[C:12]([S:11][CH:8]([CH3:10])[CH3:9])=[N:13][CH:14]=[CH:15][CH:16]=1)[CH3:5]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 95576Methyl 2-bromopropionateHCID 199579323-Pyridinol, 2-[(1-methylethyl)thio]-

生成物 1

HCID 544930632-(2-Isopropylthiopyrid-3-yloxy)-propionic acid methyl ester

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

12.3 ml of 2-bromopropionic acid methyl ester are added dropwise at room temperature to a mixture of 16.9 g of 2-isopropylthio-3-hydroxypyridine and 15.2 g of potassium carbonate in 250 ml of dimethylformamide and the batch is stirred for 75 minutes. The suspension is introduced into a mixture of ice-water (300 ml), 50 ml of 2N hydrochloric acid and 300 ml of ethyl acetate, washed four times with 120 ml of water and 120 ml of ethyl acetate each time, and the organic phase is dried over sodium sulfate and concentrated by evaporation. 25.4 g of the desired intermediate are obtained in the form of a viscous oil.

後処理

  1. washwashed four times with 120 ml of water and 120 ml of ethyl acetate each time
  2. dry with materialthe organic phase is dried over sodium sulfate
  3. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-cb746f3e77cc4c7ca2fa00427cf9c504
出典データセット
uspto-grants-1997_04
特許番号
US05625071

関連ノート

読み込み中…