Tetrahydrofuran → 4-(3-Chloro-1,4-dihydro-1,4-dioxo-2-naphthalenyl)-1-piperazinecarboxylic acid, 2-methylpropyl ester

HRID 622392

反応式

HRID 622392 の反応式
[Cl:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:13])[C:3]=1[N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1.Cl[C:21]([O:23][CH2:24][CH2:25][CH2:26]C)=[O:22].O1CCC[CH2:29]1>>[Cl:1][C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:13])[C:3]=1[N:14]1[CH2:19][CH2:18][N:17]([C:21]([O:23][CH2:24][CH:25]([CH3:26])[CH3:29])=[O:22])[CH2:16][CH2:15]1

参加物

4

反応物 3

HCID 8028Tetrahydrofuran2 回HCID 61140Butyl chloroformateHCID 6997941,4-Naphthalenedione, 2-chloro-3-(1-piperazinyl)-

生成物 1

HCID 139347664-(3-Chloro-1,4-dihydro-1,4-dioxo-2-naphthalenyl)-1-piperazinecarboxylic acid, 2-methylpropyl ester

実験手順

A solution of 830 mg of 3-chloro-2-piperazinyl 1,4-naphthoquinone in 50 ml of tetrahydrofuran was added dropwise to a solution of 0.39 ml of butyl chloroformate in 10 ml of tetrahydrofuran. This mixture was stirred for 20 minutes, then filtered and the filtrate concentrated to an oil. The oil was crystallized from ether/hexane, giving 360 mg of the desired product, mp 92-94°C.

後処理

  1. filtrationfiltered
  2. concentrationthe filtrate concentrated to an oil
  3. customThe oil was crystallized from ether/hexane

出典と根拠

ORDレコード
ord-787442818321466eb57083b50903aa55
出典データセット
uspto-grants-1988_09
特許番号
US04771061

関連ノート

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