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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0

홈
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Ethyl Acetate → 4-(3-Chloro-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

HRID 1993638

인쇄 미리보기

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HRID 1993638 반응식

Cl[C:2]1[C:7]([Cl:8])=[CH:6][C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=1.[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:14])[CH3:13].C(=O)([O-])[O-].[K+].[K+].C(OCC)(=O)C>CN(C=O)C.O>[C:12]([O:16][C:17]([N:19]1[CH2:24][CH2:23][N:22]([C:2]2[C:7]([Cl:8])=[CH:6][C:5]([N+:9]([O-:11])=[O:10])=[CH:4][N:3]=2)[CH2:21][CH2:20]1)=[O:18])([CH3:15])([CH3:13])[CH3:14]

참가 물질 반응 조건 실험 절차 후처리 출처 및 근거 반응 노트

참가 물질

7

반응물 4

HCID 8857Ethyl Acetate

HCID 11430Potassium Carbonate

HCID 143452tert-Butyl piperazine-1-carboxylate

HCID 27631062,3-Dichloro-5-nitropyridine

생성물 1

HCID 685401434-(3-Chloro-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester수율 93%

시약·촉매·용매 2

HCID 962

Water

용매

HCID 6228Dimethylformamide용매

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온도: 80 °C

실험 절차

Place 2,3-dichloro-5-nitro-pyridine (2.0 g, 10.36 mmol), piperazine-1-carboxylic acid tert-butyl ester (2.12 g, 11.40 mmol), and potassium carbonate (1.72 g, 12.43 mmol) in DMF (20 mL). Heat to 80° C. for 2.5 days. Cool to room temperature and add ethyl acetate and water. Separate organic layer and wash with water and saturated aq. sodium chloride. Collect organic layer, dry over Mg2SO4, filter, and concentrate under reduced pressure. Subject residue to silica gel chromatography eluting with 20% EtOAc:hexane to yield 3.29 g (93%) of 4-(3-chloro-5-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester. MS(ES): m/z=341 [M+H].

후처리

temperatureCool to room temperature
washSeparate organic layer and wash with water and saturated aq. sodium chloride
dry with materialCollect organic layer, dry over Mg2SO4
filtrationfilter
concentrationconcentrate under reduced pressure
washSubject residue to silica gel chromatography eluting with 20% EtOAc

출처 및 근거

ORD 기록: ord-ddb6dec00f7f4fdab871ea617e4a4de5
출처 데이터셋: uspto-grants-2010_01
DOI: 10.6084/m9.figshare.5104873.v1
특허 번호: US07652015B2

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