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Methanol → HCID 54364994, 화합물

HRID 1646466
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HRID 1646466 반응식
[NH2:1][C:2]1[C:3]([F:16])=[CH:4][C:5]([Cl:15])=[C:6]([S:8][C:9]2([C:12]([OH:14])=[O:13])[CH2:11][CH2:10]2)[CH:7]=1.[CH3:17]O>S(=O)(=O)(O)O>[CH3:17][O:13][C:12]([C:9]1([S:8][C:6]2[CH:7]=[C:2]([NH2:1])[C:3]([F:16])=[CH:4][C:5]=2[Cl:15])[CH2:11][CH2:10]1)=[O:14]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 887MethanolHCID 198006261-(5-Amino-2-chloro-4-fluorophenylthio)-cyclopropanecarboxylic acid

생성물 1

HCID 54364994HCID 54364994, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid촉매

실험 절차

A solution of 3.6 g of 1-(5-amino-2-chloro-4-fluorophenylthio)-cyclopropanecarboxylic acid and a few drops of sulfuric acid in 50 ml of methanol is heated under reflux until the starting material can no longer be detected. The methanol is then evaporated off, water and ethyl acetate are added to the residue and the organic phase is washed in succession with sodium hydrogen carbonate solution, water and saturated sodium chloride solution. Concentration and purification of the crude product by means of silica gel chromatography yield 5.7 g of 1-(5-amino-2-chloro-4-fluorophenylthio)-cyclopropanecarboxylic acid methyl ester having a melting point of from +119° to +121° C.

후처리

  1. temperatureunder reflux until the starting material
  2. customThe methanol is then evaporated off
  3. additionwater and ethyl acetate are added to the residue
  4. washthe organic phase is washed in succession with sodium hydrogen carbonate solution, water and saturated sodium chloride solution
  5. concentrationConcentration and purification of the crude product by means of silica gel chromatography yield 5.7 g of 1-(5-amino-2-chloro-4-fluorophenylthio)-cyclopropanecarboxylic acid methyl ester having a melting point of from +119° to +121° C.

출처 및 근거

ORD 기록
ord-e62f18c31d874f4b8141c63cea525f38
출처 데이터셋
uspto-grants-1993_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05180418

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