Methanol → HCID 69889855、化合物

HRID 2119438ノート

反応式

HRID 2119438 の反応式
[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

参加物

5

反応物 4

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

生成物 1

HCID 69889855HCID 69889855、化合物収率 90%

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-fa74d8e88dd6465db1938a8b3a76cce3
出典データセット
uspto-grants-2004_02
特許番号
US06686368B1

反応ノート

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