4-Acetylbenzoic acid p-nitrophenyl ester → HCID 15895998、化合物

HRID 1954192ノート

反応式

HRID 1954192 の反応式
[N+](C1C=CC(O[C:11](=[O:21])[C:12]2[CH:17]=[CH:16][C:15]([C:18](=[O:20])[CH3:19])=[CH:14][CH:13]=2)=CC=1)([O-])=O.[NH2:22][C:23]1[S:24][CH:25]=[C:26]([C:28]([NH:30][CH2:31][CH2:32][N:33]([CH:37]([CH3:39])[CH3:38])[CH:34]([CH3:36])[CH3:35])=[O:29])[N:27]=1>>[C:18]([C:15]1[CH:14]=[CH:13][C:12]([C:11]([NH:22][C:23]2[S:24][CH:25]=[C:26]([C:28]([NH:30][CH2:31][CH2:32][N:33]([CH:37]([CH3:39])[CH3:38])[CH:34]([CH3:35])[CH3:36])=[O:29])[N:27]=2)=[O:21])=[CH:17][CH:16]=1)(=[O:20])[CH3:19]

参加物

3

反応物 2

HCID 158959964-Acetylbenzoic acid p-nitrophenyl esterHCID 158959972-Amino-4-[(2-diisopropylaminoethyl)aminocarbonyl]-1,3-thiazole

生成物 1

HCID 15895998HCID 15895998、化合物収率 57.1%

反応条件

温度
130 °C

実験手順

To 831 mg of 4-acetylbenzoic acid p-nitrophenyl ester, 788 mg of 2-amino-4-[(2-diisopropylaminoethyl)aminocarbonyl]-1,3-thiazole were added. The resulting mixture was stirred at 130° C. for 8 hours. The reaction mixture was purified by column chromatography on NH silica gel (chloroform), whereby 693 mg of 2-[N-(4-acetylbenzoyl)amino]-4-[(2-diisopropylaminoethyl)aminocarbonyl]-1,3-thiazole were obtained. After 2 ml of a 4N hydrochloric acid--dioxane solution were added to the resulting compound, the solvent was distilled off under reduced pressure. The residue was recrystallized from a mixed solvent of isopropyl ether and ethanol, whereby 395 mg of the title compound were obtained as yellow powder.

後処理

  1. customThe reaction mixture was purified by column chromatography on NH silica gel (chloroform)

出典と根拠

ORDレコード
ord-ea2b3a078ac04453be0439eb19303e32
出典データセット
uspto-grants-2000_09
特許番号
US06121301

反応ノート

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