4-(Methylsulfonyl)benzaldehyde → HCID 70286603, 화합물

HRID 377761

반응식

HRID 377761 반응식
C[O-].[Na+].[CH3:4][O:5][C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)[CH2:11][C:10]([CH3:15])=[C:9]2[CH2:16][C:17]([O:19]C)=[O:18].[CH3:21][S:22]([C:25]1[CH:32]=[CH:31][C:28]([CH:29]=O)=[CH:27][CH:26]=1)(=[O:24])=[O:23]>O>[CH3:4][O:5][C:6]1[CH:7]=[C:8]2[C:12](=[CH:13][CH:14]=1)/[C:11](=[CH:29]\[C:28]1[CH:31]=[CH:32][C:25]([S:22]([CH3:21])(=[O:24])=[O:23])=[CH:26][CH:27]=1)/[C:10]([CH3:15])=[C:9]2[CH2:16][C:17]([OH:19])=[O:18]

참가 물질

5

반응물 3

HCID 2203764-(Methylsulfonyl)benzaldehydeHCID 10942334Sodium MethoxideHCID 53634864HCID 53634864, 화합물

생성물 1

HCID 70286603HCID 70286603, 화합물

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

25% methanolic sodium methoxide (16 ml, 2.0 equivalents) is treated with a solution of methyl 5-methoxy-2-methyl-3-indenylacetate (from Example 4, Part C) (8.7 g; 0.037 mol) and p-methylsulfonylbenzaldehyde, (6.3 g; 1.1 equivalent). The mixture is stirred at reflux under nitrogen for 2 hours. An equal volume of water is added slowly, and refluxing is continued for 30 min. The solution is cooled, is diluted with water and is washed with ether. Residual ether is blown off with nitrogen. The aqueous solution is acidified with 10% hydrochloric acid. The precipitated product is collected and is washed thoroughly with water. The crude product is crystallized from methanol to give (Z)-5-methoxy-2-methyl-1-(p-methylsulfonylbenzylidene)-3-indenylacetic acid.

후처리

  1. temperatureat reflux under nitrogen for 2 hours
  2. temperaturerefluxing
  3. temperatureThe solution is cooled
  4. washis washed with ether
  5. customThe precipitated product is collected
  6. washis washed thoroughly with water
  7. customThe crude product is crystallized from methanol

출처 및 근거

ORD 기록
ord-113586e271734fa8a1342d6dff985c0c
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028116

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