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Sodium Chloride → 4-(3-Oxo-3,4-dihydro-quinoxalin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

HRID 1295704
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인쇄 미리보기

반응식

HRID 1295704 반응식
[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:23](Cl)=[N:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].[OH-:25].[Na+].[Cl-].[Na+]>C(OC)(C)(C)C.O.CS(C)=O>[C:1]([O:5][C:6]([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[C:23](=[O:25])[NH:22][C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[N:15]=2)[CH2:10][CH2:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 5234Sodium ChlorideHCID 14798Sodium HydroxideHCID 45788978tert-Butyl 4-(3-chloroquinoxalin-2-yl)piperazine-1-carboxylate

생성물 1

HCID 693660094-(3-Oxo-3,4-dihydro-quinoxalin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

시약·촉매·용매 3

HCID 679Dimethyl Sulfoxide용매
HCID 962
Water
용매
2회
HCID 15413tert-Butyl methyl ether용매

실험 절차

4-(3-Chloro-quinoxalin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (10.0 g, 28.7 mmol; from Step 1) was added to a mixture of sodium hydroxide (40 g), water (40 g) and DMSO (40 g) at 100° C. After being stirred for 1 h at this temperature, water (200 g) and methyl tert-butyl ether (1000 g) and sodium chloride (50 g) were added. The crystals formed from the organic layer were collected by filtration and dried. This furnished 4.0 g (42%) of the title compound as white crystals. 1H NMR analysis supports the stated structure.

후처리

  1. additionwere added
  2. customThe crystals formed from the organic layer
  3. filtrationwere collected by filtration
  4. customdried

출처 및 근거

ORD 기록
ord-61b912565ff947caaa3f87b86d17c617
출처 데이터셋
uspto-grants-2007_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07244722B2

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