Potassium Carbonate → 2-[1-(4-chlorobenzyl)-1H-indol-3-yl]-2-oxo-N-(5-oxo-2,5-dihydro-3-thienyl)acetamide

HRID 353475노트

반응식

HRID 353475 반응식
[NH2:1][C:2]1[CH2:6][S:5][C:4](=[O:7])[CH:3]=1.COC1C=C2C(=C(OC)C=1)N(CC1C=CC(Cl)=CC=1)C=C2.C(=O)([O-])[O-].[K+].[K+].[Cl:35][C:36]1[CH:56]=[CH:55][C:39]([CH2:40][N:41]2[C:49]3[C:44](=[CH:45][CH:46]=[CH:47][CH:48]=3)[C:43]([C:50](=[O:54])[C:51](Cl)=[O:52])=[CH:42]2)=[CH:38][CH:37]=1>COCCOC.O>[Cl:35][C:36]1[CH:56]=[CH:55][C:39]([CH2:40][N:41]2[C:49]3[C:44](=[CH:45][CH:46]=[CH:47][CH:48]=3)[C:43]([C:50](=[O:54])[C:51]([NH:1][C:2]3[CH2:6][S:5][C:4](=[O:7])[CH:3]=3)=[O:52])=[CH:42]2)=[CH:38][CH:37]=1

참가 물질

7

반응물 4

HCID 11430Potassium CarbonateHCID 109804772-(1-(4-chlorobenzyl)-1H-indol-3-yl)-2-oxo-acetyl chlorideHCID 222568845,7-Dimethoxy-1-(4-chlorobenzyl)indoleHCID 235140804-amino-5H-thiophen-2-one

생성물 1

HCID 235140422-[1-(4-chlorobenzyl)-1H-indol-3-yl]-2-oxo-N-(5-oxo-2,5-dihydro-3-thienyl)acetamide

시약·촉매·용매 2

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매

실험 절차

A suspension of 4-amino-5H-thiophen-2-one of Preparation 5 (103 mg), powdered potassium carbonate (138 mg) and 2-(1-(4-chlorobenzyl)-1H-indol-3-yl)-2-oxo-acetyl chloride of Example 1 (334 mg) in 1,2-dimethoxyethane (5 ml) is stirred at room temperature for 2 h. After this time the reaction mixture is poured in water (50 ml) and the obtained precipitate is collected by filtration and thoroughly washed with water. The still wet solid is suspended in methanol and stirred for 30′. Filtration followed by drying at 40° C. under vacuum gives 2-[1-(4-chlorobenzyl)-1H-indol-3-yl]-2-oxo-N-(5-oxo-2,5-dihydro-3-thienyl)acetamide (280 mg).

후처리

  1. filtrationthe obtained precipitate is collected by filtration
  2. washthoroughly washed with water
  3. stirringstirred for 30′
  4. filtrationFiltration
  5. customby drying at 40° C. under vacuum

출처 및 근거

ORD 기록
ord-2b4124f0d6124809b3de884b5fbdbcec
출처 데이터셋
uspto-grants-2004_06
특허 번호
US06753342B2

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