Methanol → HCID 69500037, 화합물

HRID 2207947노트

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HRID 2207947 반응식
C[O:2][C:3]([C:5]1[CH2:9][CH:8]([C:10]2[S:11][C:12]([Br:15])=[CH:13][CH:14]=2)[N:7]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[Cl:22])[N:6]=1)=[O:4].[OH-].[K+].CO>O>[Br:15][C:12]1[S:11][C:10]([CH:8]2[N:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[Cl:22])[N:6]=[C:5]([C:3]([OH:4])=[O:2])[CH2:9]2)=[CH:14][CH:13]=1

참가 물질

5

반응물 3

HCID 887MethanolHCID 14797Potassium HydroxideHCID 118432122HCID 118432122, 화합물

생성물 1

HCID 69500037HCID 69500037, 화합물수율 99.2%

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

5-(5-Bromo-thiophen-2-yl)-1-(2-chloro-phenyl)-4,5-dihydro-1H-pyrazole-3-carboxylic acid methyl ester (18.9 g, 47.3 mmol) prepared in Step 3 and a solution of potassium hydroxide (5.3 g, 94.6 mmol) in distilled water (200.0 mL) were added to methanol (200.0 mL). The reaction mixture was stirred at 80° C. for 12 hours and then concentrated under reduced pressure to discard methanol. The resulting residue was washed with diethyl ether, acidified by a 1N hydrochloric acid solution, and then extracted with ethyl acetate. The extract was washed with distilled water and brine, dried on anhydrous magnesium sulfate, and then concentrated under reduced pressure to give 18.1 g of the titled compound as a pale yellow solid.

후처리

  1. concentrationconcentrated under reduced pressure
  2. washThe resulting residue was washed with diethyl ether
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with distilled water and brine
  5. dry with materialdried on anhydrous magnesium sulfate
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-4e2546411266489891ecc2fb23ba5922
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376420B2

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