4-(Methylsulfonyl)benzaldehyde → HCID 70288307, 화합물

HRID 377758

반응식

HRID 377758 반응식
[CH3:1][S:2]([C:5]1[CH:12]=[CH:11][C:8]([CH:9]=O)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[CH3:13][N:14]([CH3:30])[C:15]1[CH:16]=[C:17]2[C:21](=[CH:22][CH:23]=1)[CH2:20][C:19]([CH3:24])=[C:18]2[CH2:25][C:26]([O:28]C)=[O:27].CC(C)([O-])C.[K+]>COCCOC.CCOCC>[CH3:1][S:2]([C:5]1[CH:12]=[CH:11][C:8](/[CH:9]=[C:20]2/[C:19]([CH3:24])=[C:18]([CH2:25][C:26]([OH:28])=[O:27])[C:17]3[C:21]/2=[CH:22][CH:23]=[C:15]([N:14]([CH3:30])[CH3:13])[CH:16]=3)=[CH:7][CH:6]=1)(=[O:4])=[O:3]

참가 물질

6

반응물 3

HCID 2203764-(Methylsulfonyl)benzaldehydeHCID 22456970HCID 22456970, 화합물HCID 23665647Potassium tert-butoxide

생성물 1

HCID 70288307HCID 70288307, 화합물

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 80711,2-Dimethoxyethane용매

실험 절차

p-Methylsulfonylbenzaldehyde (1.5 g) is added to a solution of methyl 5-dimethylamino-2-methyl-3-indenylacetate (2.5 g) from Example 3 Part B in 1,2-dimethoxyethane (1.5 ml) at 0° C. followed by the addition of potassium t-butoxide (1.1 g). The reaction mixture is kept in the ice-bath for 4 hours and at room temperature for 18 hours. The mixture is diluted with ether (15 ml), and the potassium salt is filtered off. The salt is dissolved in 30 ml of water and neutralized with dilute hydrochloric acid to pH 6-6.5. The crude acid precipitates, is collected by filtration and is recrystallized to give pure (Z)-1-(p-methylsulfonylbenzylidene)-5-dimethylamino-2-methyl-3-indenylacetic acid.

후처리

  1. filtrationthe potassium salt is filtered off
  2. dissolutionThe salt is dissolved in 30 ml of water and neutralized with dilute hydrochloric acid to pH 6-6.5
  3. customThe crude acid precipitates
  4. filtrationis collected by filtration
  5. customis recrystallized

출처 및 근거

ORD 기록
ord-5986da5bcbb94caca87cddaa171c9d2b
출처 데이터셋
uspto-grants-2000_02
특허 번호
US06028116

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