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

HRID 1788906노트

반응식

HRID 1788906 반응식
[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

참가 물질

4

반응물 3

HCID 8028Tetrahydrofuran2회HCID 61140Butyl chloroformateHCID 6997941,4-Naphthalenedione, 2-chloro-3-(1-piperazinyl)-

생성물 1

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

실험 절차

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 recrystallized from ether/hexane, giving 360 mg of the desired product, mp 92°-94° C.

후처리

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

출처 및 근거

ORD 기록
ord-da7582724371467fa51419dee56b16ee
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04686220

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