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Benzoyl chloride → 1-Benzoyl-1,2,4,7-tetrahydro-5-methyl-7-(3-nitrophenyl)-2-oxopyrazolo[1,5-a]pyrimidine-6-carboxylic acid, 1-methylethyl ester

HRID 1252992
ノート
印刷プレビュー

反応式

HRID 1252992 の反応式
[CH3:1][C:2]1[NH:3][C:4]2[N:5]([NH:23][C:24](=[O:26])[CH:25]=2)[CH:6]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:7]=1[C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9].[C:27](Cl)(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1>ClCCl.N1C=CC=CC=1.C(OCC)(=O)C>[C:27]([N:23]1[N:5]2[CH:6]([C:14]3[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=3)[C:7]([C:8]([O:10][CH:11]([CH3:13])[CH3:12])=[O:9])=[C:2]([CH3:1])[NH:3][C:4]2=[CH:25][C:24]1=[O:26])(=[O:34])[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 7412Benzoyl chlorideHCID 141304321,2,4,7-Tetrahydro-5-methyl-7-(3-nitrophenyl)-2-oxopyrazolo[1,5-a]pyrimdine-6-carboxylic acid, 1-methylethyl ester

生成物 1

HCID 141304341-Benzoyl-1,2,4,7-tetrahydro-5-methyl-7-(3-nitrophenyl)-2-oxopyrazolo[1,5-a]pyrimidine-6-carboxylic acid, 1-methylethyl ester

試薬・触媒・溶媒 3

HCID 1049Pyridine溶媒
HCID 6344
Dichloromethane
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

A suspension of 1,2,4,7-tetrahydro-5-methyl-7-(3-nitrophenyl)-2-oxopyrazolo[1,5-a]pyrimidine-6-carboxylic acid, 1-methylethyl ester (36 mg; 0.1 mmole) in dichloromethane (2 ml) and pyridine (1 ml) under argon was treated with benzoyl chloride (28 mg; 0.2 mmole). The reaction was allowed to stir for 30 minutes and then diluted with ethyl acetate. The resulting solution was washed with 1N hydrochloric acid, water, sodium bicarbonate and brine. It was dried over anhydrous magnesium sulfate and evaporated. The residue was purified by preparative thin layer chromatography (40% acetone in hexanes) and the product was crystallized from absolute ethanol to provide a solid, melting point 201°-203° C.

後処理

  1. washThe resulting solution was washed with 1N hydrochloric acid, water, sodium bicarbonate and brine
  2. dry with materialIt was dried over anhydrous magnesium sulfate
  3. customevaporated
  4. customThe residue was purified by preparative thin layer chromatography (40% acetone in hexanes)
  5. customthe product was crystallized from absolute ethanol
  6. customto provide a solid, melting point 201°-203° C.

出典と根拠

ORDレコード
ord-1f55c69efeed4bbdb5bf140c72cebad0
出典データセット
uspto-grants-1988_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04746656

反応ノート

読み込み中…

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