1-Hydroxybenzotriazole → HCID 18331075, 화합물

HRID 2270055노트

반응식

HRID 2270055 반응식
Cl.[NH2:2][CH2:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:8][CH:7]=1)=[O:5].[CH2:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:35]=[CH:34][C:30]([C:31](O)=[O:32])=[CH:29][CH:28]=2)=[CH:23][CH:22]=1)[CH2:18][CH3:19].ON1C2C=CC=CC=2N=N1.Cl.C(N=C=NCCCN(C)C)C>C(N(CC)CC)C.ClCCl.O>[CH2:17]([O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]2[CH:35]=[CH:34][C:30]([C:31]([NH:2][CH2:3][C:4]([C:6]3[CH:11]=[CH:10][C:9]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:8][CH:7]=3)=[O:5])=[O:32])=[CH:29][CH:28]=2)=[CH:23][CH:22]=1)[CH2:18][CH3:19]

참가 물질

8

반응물 4

HCID 757711-HydroxybenzotriazoleHCID 20636134-(4-propoxyphenyl)benzoic AcidHCID 27239391,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochlorideHCID 18613865193813-77-3

생성물 1

HCID 18331075HCID 18331075, 화합물수율 58.3%

시약·촉매·용매 3

HCID 962Water용매HCID 6344Dichloromethane용매HCID 8471Triethylamine용매

실험 절차

To a solution of 2-amino-4′-ethoxycarbonylacetophenone hydrochloride (700 mg), 4-(4-propoxyphenyl)benzoic acid (866 mg) and 1-hydroxybenzotriazole (456.5 mg) in triethylamine (0.47 ml) and dichloromethane (7 ml) was added 1-ethyl-3-(3′-dimethylaminopropyl)carbodiimide hydrochloride (WSC.HCl) (648 mg), and stirred for 5 hours at ambient temperature. To the reaction mixture was added water (100 ml), and extracted with dichloromethane. The organic layer was washed with 1N hydrochloric acid, water, saturated sodium hydrogen carbonate aqueous solution and brine. Then the organic layer was dried over magnesium sulfate. Magnesium sulfate was filtered off, and the filtrate was evaporated under reduced pressure. The solids were slurried in ethyl acetate, and collected by filtration to give 2-[4-(4-propoxyphenyl)benzoylamino]-4′-ethoxycarbonylacetophenone (746 mg).

후처리

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with 1N hydrochloric acid, water, saturated sodium hydrogen carbonate aqueous solution and brine
  3. dry with materialThen the organic layer was dried over magnesium sulfate
  4. filtrationMagnesium sulfate was filtered off
  5. customthe filtrate was evaporated under reduced pressure
  6. filtrationcollected by filtration

출처 및 근거

ORD 기록
ord-b1edf2820aa444a0b1f5d7cd3f20fc10
출처 데이터셋
uspto-grants-2001_12
특허 번호
US06331521B1

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