1-Hydroxybenzotriazole → HCID 18331075、化合物

HRID 2270055ノート

反応式

HRID 2270055 の反応式
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]

参加物

8

反応物 4

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

生成物 1

HCID 18331075HCID 18331075、化合物収率 58.3%

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6344Dichloromethane溶媒HCID 8471Triethylamine溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-b1edf2820aa444a0b1f5d7cd3f20fc10
出典データセット
uspto-grants-2001_12
特許番号
US06331521B1

反応ノート

読み込み中…