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

HRID 55549

반응식

HRID 55549 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cb746f3e77cc4c7ca2fa00427cf9c504
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05625071

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