Lithium Hydroxide → HCID 67020984、化合物

HRID 12912ノート

反応式

HRID 12912 の反応式
C([O:3][C:4]([C:6]1[CH:7]=[N:8][N:9]([CH2:15][CH:16]2[CH2:18][CH2:17]2)[C:10]=1[C:11]([F:14])([F:13])[F:12])=[O:5])C.[Li+].[OH-]>CO.O>[CH:16]1([CH2:15][N:9]2[C:10]([C:11]([F:12])([F:13])[F:14])=[C:6]([C:4]([OH:5])=[O:3])[CH:7]=[N:8]2)[CH2:18][CH2:17]1

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 670209131-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester

生成物 1

HCID 67020984HCID 67020984、化合物収率 93%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 1-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid ethyl ester (120 mg, 0.46 mmol) in methanol (5 mL) and water (5 mL) was added LiOH (13 mg, 0.54 mmol). The reaction mixture was stirred at reflux overnight, and then the solution was concentrated under reduced pressure to remove the methanol. The residue was diluted with water and the solution was acidified to pH=2 with concentrated HCL. The resulting mixture was then extracted with ethyl acetate three times. The combined organic layers were concentrated in vacuo to give 1-cyclopropylmethyl-5-trifluoromethyl-1H-pyrazole-4-carboxylic acid (100 mg, 93%), which was used without further purification.

後処理

  1. temperatureat reflux overnight
  2. concentrationthe solution was concentrated under reduced pressure
  3. customto remove the methanol
  4. additionThe residue was diluted with water
  5. extractionThe resulting mixture was then extracted with ethyl acetate three times
  6. concentrationThe combined organic layers were concentrated in vacuo

出典と根拠

ORDレコード
ord-b7f5194d744d48d4a0c4411e09c0c4d1
出典データセット
uspto-grants-2010_06
特許番号
US07728029B2

反応ノート

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