Dimethylamine, hydrochloride → N-(1-Acetyl-5-dimethylaminomethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide

HRID 1107943노트

반응식

HRID 1107943 반응식
[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:23])[C:9]([CH2:21]Cl)=[C:10]([CH3:20])[C:11]=2[NH:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[CH2:6][CH2:5]1)(=[O:3])[CH3:2].[NH:24]([CH3:26])[CH3:25].Cl.C([O-])([O-])=O.[K+].[K+]>C(Cl)(Cl)Cl>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:23])[C:9]([CH2:21][N:24]([CH3:26])[CH3:25])=[C:10]([CH3:20])[C:11]=2[NH:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[CH2:6][CH2:5]1)(=[O:3])[CH3:2]

참가 물질

5

반응물 3

HCID 10473Dimethylamine, hydrochlorideHCID 11430Potassium CarbonateHCID 15895572N-(1-Acetyl-5-chloromethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide

생성물 1

HCID 22247311N-(1-Acetyl-5-dimethylaminomethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide수율 34.1%

시약·촉매·용매 1

HCID 6212Chloroform용매2회

실험 절차

N-(1-Acetyl-5-chloromethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide (2.0 g) was dissolved in CHCl3 (40 ml) and (CH3)2NH.HCl (3.5 g) and K2CO3 (11.8 g) were added, which was followed by stirring at room temperature for 4 hr. CHCl3 (300 ml) was added, and the mixture was washed successively with 2N-hydrochloric acid, 2N aqueous NaOH and saturated brine, and dried over anhydrous sodium sulfate. CHCl3 was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=10/1-1/1) to give 700 mg of N-(1-acetyl-5-dimethylaminomethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide.

후처리

  1. washthe mixture was washed successively with 2N-hydrochloric acid, 2N aqueous NaOH and saturated brine
  2. dry with materialdried over anhydrous sodium sulfate
  3. customCHCl3 was evaporated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: CHCl3 /MeOH=10/1-1/1)

출처 및 근거

ORD 기록
ord-d96a158f2fb1416886ac9a2b2eb716eb
출처 데이터셋
uspto-grants-2000_05
특허 번호
US06063806

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