Methanol → HCID 69889855, 화합물

HRID 2085018노트

반응식

HRID 2085018 반응식
[CH3:1][C:2]1[CH:6]=[C:5](C(OCC)=O)[N:4]([C:12]2[C:21]([F:22])=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:13]=2)[N:3]=1.O[Li].[OH2:25].[OH2:26].[CH3:27]O>>[CH3:27][C:2]1([C:1]([OH:26])=[O:25])[CH:6]=[CH:5][N:4]([C:12]2[C:21]([F:22])=[CH:20][C:19]3[C:14](=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH:13]=2)[NH:3]1

참가 물질

5

반응물 4

HCID 887MethanolHCID 962WaterHCID 168937Lithium hydroxide, monohydrateHCID 22728901ethyl 3-methyl-1-(3-fluoro-2-naphthyl)-1H-pyrazole-5-carboxylate

생성물 1

HCID 69889855HCID 69889855, 화합물수율 90%

실험 절차

The preparation of ethyl 3-methyl-1-(3-fluoro-2-naphthyl)-1H-pyrazole-5-carboxylate was the same as that in Step 3 for Example 3. This ester (13.2 g, 44 mmol) was dissolved in 80 mL methanol. To it were added LiOH.H2O (3.7 g, 49 mmol) and 40 mL water. The mixture was stirred for overnight at room temperature. It was evaporated in vacuuo to remove methanol. The residue was acidified with 1N HCl till pH 1. The mixture was extracted with EtOAc (×4). The organic extracts were combined, dried, evaporated and pumped to dryness to afford 3-methyl-1-(3-fluoro-2-naphthyl)-1H-pyrazolecarboxylic acid in over 90% yield. ES-MS: (M+H)+ 271.

후처리

  1. customIt was evaporated in vacuuo
  2. customto remove methanol
  3. extractionThe mixture was extracted with EtOAc (×4)
  4. customdried
  5. customevaporated

출처 및 근거

ORD 기록
ord-43e6efc6328049508b185a81c7f1efd1
출처 데이터셋
uspto-grants-2004_04
특허 번호
US06720317B1

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