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

HRID 1531953ノート

反応式

HRID 1531953 の反応式
[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].Cl.C([O-])([O-])=O.[K+].[K+].[NH:31]([CH3:33])[CH3:32]>C(Cl)(Cl)Cl>[C:1]([N:4]1[C:12]2[C:7](=[C:8]([CH3:23])[C:9]([CH2:21][N:31]([CH3:33])[CH3:32])=[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]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 674DimethylamineHCID 11430Potassium CarbonateHCID 15895572N-(1-Acetyl-5-chloromethyl-4,6-dimethylindolin-7-yl)-2,2-dimethylpropanamide

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

N-(1-Acetyl-5-chloromethyl-4,6-dimethylindolin-7-yl)-2,2-dimethyl-propanamide (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.

後処理

  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)

出典と根拠

ORDレコード
ord-de62202ade7243c0addaaf54efdeb66e
出典データセット
uspto-grants-2001_03
特許番号
US06200988B1

反応ノート

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