Formic Acid → HCID 67252161、化合物

HRID 912581ノート

反応式

HRID 912581 の反応式
C[O:2][C:3]([C:5]1[C:9]([CH3:10])=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]([F:20])([F:19])[F:18])[N:7]([CH3:21])[CH:6]=1)=[O:4].[OH-].[Na+].C(O)=O>CO.O>[CH3:21][N:7]1[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][C:12]=2[C:17]([F:19])([F:20])[F:18])=[C:9]([CH3:10])[C:5]([C:3]([OH:4])=[O:2])=[CH:6]1

参加物

6

反応物 3

HCID 284Formic AcidHCID 14798Sodium HydroxideHCID 67253051HCID 67253051、化合物

生成物 1

HCID 67252161HCID 67252161、化合物収率 90.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 1,4-dimethyl-5-(2-trifluoromethyl-phenyl)-1H-pyrrole-3-carboxylic acid methyl ester (2.5 g, 8.4 mmol) in MeOH (20 mL) was added 4N NaOH (10 mL) and the mixture was heated to reflux overnight. Evaporation of solvent gave a solid, which was re-dissolved in water. The solution was acidified with formic acid. The resulting solids were collected by filtration, washed with water and then dried under high vacuum to afford the title compound as an off-white solid (2.15 g, 90%). MS (ES): 284 (MH+).

後処理

  1. temperaturethe mixture was heated
  2. temperatureto reflux overnight
  3. customEvaporation of solvent
  4. customgave a solid, which
  5. filtrationThe resulting solids were collected by filtration
  6. washwashed with water
  7. customdried under high vacuum

出典と根拠

ORDレコード
ord-0ed749bdbc9f41ab8b66d1d039d816ae
出典データセット
uspto-grants-2011_09
特許番号
US08026237B2

反応ノート

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