Water → HCID 70288966、化合物

HRID 377757

反応式

HRID 377757 の反応式
[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])[CH2:7][C:6]([CH3:12])=[C:5]2[CH2:13][C:14]([O:16]C)=[O:15].[CH3:18][S:19]([C:22]1[CH:29]=[CH:28][C:25]([CH:26]=O)=[CH:24][CH:23]=1)(=[O:21])=[O:20].O>N1C=CC=CC=1>[F:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[F:11])/[C:7](=[CH:26]\[C:25]1[CH:24]=[CH:23][C:22]([S:19]([CH3:18])(=[O:21])=[O:20])=[CH:29][CH:28]=1)/[C:6]([CH3:12])=[C:5]2[CH2:13][C:14]([OH:16])=[O:15]

参加物

5

反応物 3

HCID 962Water2 回HCID 2203764-(Methylsulfonyl)benzaldehydeHCID 12052144HCID 12052144、化合物

生成物 1

HCID 70288966HCID 70288966、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

Methyl 5,6-difluoro-2-methylindene-3-acetate (1.19 g, 5.0 mmol) from Example 2, Part E and of p-methylsulfonylbenzaldehyde (0.76 g, 5.0 mmol) in dry pyridine (10 ml) are treated under nitrogen with Triton B (5.0 g, 5.1 mmol). The deeply colored solution is kept overnight. Water (2 ml) is added, the solution is stirred for 15 minutes and is poured into excess water. The mixture is extracted with ether (2×50 ml). The aqueous phase is added to 10% HCl-ice. The solution of the precipitate is extracted into methylene chloride and is dried (MgSO4). The solvent is evaporated to leave an orange solid which is recrystallized from benzene to give (Z)-5,6-difluoro-2-methyl-1-(p-methylsulfonylbenzylidene)-indene-3-acetic acid.

後処理

  1. extractionThe mixture is extracted with ether (2×50 ml)
  2. additionThe aqueous phase is added to 10% HCl-ice
  3. extractionThe solution of the precipitate is extracted into methylene chloride
  4. dry with materialis dried (MgSO4)
  5. customThe solvent is evaporated
  6. customto leave an orange solid which
  7. customis recrystallized from benzene

出典と根拠

ORDレコード
ord-5f0ad651339a4210bcd234822b133a3f
出典データセット
uspto-grants-2000_02
特許番号
US06028116

関連ノート

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