Water → HCID 70288966, 화합물

HRID 377757

반응식

HRID 377757 반응식
[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]

참가 물질

5

반응물 3

HCID 962Water2회HCID 2203764-(Methylsulfonyl)benzaldehydeHCID 12052144HCID 12052144, 화합물

생성물 1

HCID 70288966HCID 70288966, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5f0ad651339a4210bcd234822b133a3f
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028116

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