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Ethanolamine → 7-Chloro-3-[4-(2-hydroxyethylcarbamoyl)-benzyl]-4-oxo-1-phenyl-1,4-dihydro-quinoline-2-carboxylic acid methyl ester

HRID 1697073
ノート
印刷プレビュー

反応式

HRID 1697073 の反応式
[CH3:1][O:2][C:3]([C:5]1N(C2C=CC=CC=2)[C:7]2[C:12]([C:13](=[O:25])[C:14]=1[CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22]([OH:24])=O)=[CH:18][CH:17]=1)=[CH:11][CH:10]=[C:9]([Cl:26])[CH:8]=2)=[O:4].[NH2:33][CH2:34][CH2:35][OH:36].[CH:37]1[CH:38]=[CH:39][C:40]2[N:45](O)N=N[C:41]=2[CH:42]=1.CCN=C=NCCCN(C)C.CCN(C(C)C)C(C)C>C(Cl)Cl.CN(C=O)C>[CH3:1][O:2][C:3]([C:5]1[N:45]([C:40]2[CH:39]=[CH:38][CH:37]=[CH:42][CH:41]=2)[C:7]2[C:12]([C:13](=[O:25])[C:14]=1[CH2:15][C:16]1[CH:21]=[CH:20][C:19]([C:22](=[O:24])[NH:33][CH2:34][CH2:35][OH:36])=[CH:18][CH:17]=1)=[CH:11][CH:10]=[C:9]([Cl:26])[CH:8]=2)=[O:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 700EthanolamineHCID 159081-Ethyl-3-(3'-dimethylaminopropyl)carbodiimideHCID 757711-HydroxybenzotriazoleHCID 81531DiisopropylethylamineHCID 251817183-(4-Carboxybenzyl)-7-chloro-4-oxo-1-phenyl-1,4-dihydroquinoline-2-carboxylic acid methyl ester

生成物 1

HCID 25104303
7-Chloro-3-[4-(2-hydroxyethylcarbamoyl)-benzyl]-4-oxo-1-phenyl-1,4-dihydro-quinoline-2-carboxylic acid methyl ester
収率 54.5%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane溶媒

実験手順

A mixture of 3-(4-carboxybenzyl)-7-chloro-4-oxo-1-phenyl-1,4-dihydroquinoline-2-carboxylic acid methyl ester (167 mg, 0.37 mmol), 2-aminoethanol (34 mg, 0.56 mmol), HOBt (50 mg), EDCI (142 mg, 0.74 mmol) and DIPEA (0.5 mL) in DCM (10 mL) and DMF (0.4 mL) was stirred at RT for 2 h. The reaction mixture was then partitioned between water and EtOAc. The organic layer was separated, washed twice with water, dried over Na2SO4, filtered and evaporated under reduced pressure. The crude residue was purified twice by flash chromatography to afford 7-chloro-3-[4-(2-hydroxyethylcarbamoyl)-benzyl]-4-oxo-1-phenyl-1,4-dihydro-quinoline-2-carboxylic acid methyl ester (99 mg) as an off-white powder. MS=491 [M+H]+; MP=162-163.5° C.

後処理

  1. customThe reaction mixture was then partitioned between water and EtOAc
  2. customThe organic layer was separated
  3. washwashed twice with water
  4. dry with materialdried over Na2SO4
  5. filtrationfiltered
  6. customevaporated under reduced pressure
  7. customThe crude residue was purified twice by flash chromatography

出典と根拠

ORDレコード
ord-dc4fe49c454b4382864ee52f6f4a8258
出典データセット
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08163906B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート