Methyl iodide → Benzilic acid

HRID 23377

反応式

HRID 23377 の反応式
F[C:2]1[CH:19]=[CH:18][C:5]([C:6]([C:11]2[CH:16]=[CH:15][C:14](F)=[CH:13][CH:12]=2)([OH:10])[C:7]([OH:9])=[O:8])=[CH:4][CH:3]=1.[O-]CC.[Na+].[Na].CI>C(O)C>[C:7]([OH:9])(=[O:8])[C:6]([C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1)([C:5]1[CH:18]=[CH:19][CH:2]=[CH:3][CH:4]=1)[OH:10]

参加物

6

反応物 4

HCID 6328Methyl iodideHCID 2723922Sodium ethoxideHCID 5360545SodiumHCID 12068839Bis(4-fluorophenyl)(hydroxy)acetic acid

生成物 1

HCID 6463Benzilic acid

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

25.0 g (0.095 mol) of 4,4′-difluorobenzilic acid is added to freshly prepared sodium ethoxide solution containing 2.17 g (0.095 mol) of sodium and 200 ml of ethanol at 20° C. and stirred for 3 hours. The solution is evaporated to dryness, the residue is dissolved in DMF, 22.57 g (0.16 mol) of methyl iodide is added dropwise at 20° C., and the mixture is stirred for 24 hours. It is worked up and purified analogously to compound 12b. Yield: 21.06 g (80% of theory).

後処理

  1. customThe solution is evaporated to dryness
  2. dissolutionthe residue is dissolved in DMF
  3. stirringthe mixture is stirred for 24 hours
  4. custompurified analogously to compound 12b

出典と根拠

ORDレコード
ord-aef3a9165c004a55b2384744041b864a
出典データセット
uspto-grants-2005_02
特許番号
US06852728B2

関連ノート

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