홈MCP워크벤치Skills
홈워크벤치알림마이페이지
llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
  1. 홈
  2. /반응

Potassium Carbonate → tert-Butyl 4-(2-methyl-4-nitrophenyl)piperazine-1-carboxylate

HRID 1181618
노트
인쇄 미리보기

반응식

HRID 1181618 반응식
F[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[CH3:11].[N:12]1([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[CH3:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[N:15]1[CH2:14][CH2:13][N:12]([C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[CH2:17][CH2:16]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 68001Benzene, 1-fluoro-2-methyl-4-nitro-HCID 143452tert-Butyl piperazine-1-carboxylate

생성물 1

HCID 22336105tert-Butyl 4-(2-methyl-4-nitrophenyl)piperazine-1-carboxylate수율 62%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

4.65 g (3.10 mmol) of 2-fluoro-5-nitrotoluene, 6.71 g (3.60 mmol) of tert-butyl 1-piperazinecarboxylate and 10.4 g (7.50 mmol) of potassium carbonate are solubilized under an argon atmosphere, in dry DMF (50 ml), then the reaction medium is taken to 80° C. for 18 hours. The reaction medium is then cooled down using an ice bath then poured into ice-cold water. The product is extracted using 3 times 50 ml of ethyl acetate. The organic solution is dried over magnesium sulphate, followed by filtration and concentration under vacuum. Purification is then carried out by crystallization from diisopropyl ether and the solid obtained is filtered and rinsed with isopentane in order to obtain, after drying, 5.9 g of a yellow solid product (yield 62%). Melting point: 121.8-123.4° C.

후처리

  1. temperatureThe reaction medium is then cooled down
  2. additionthen poured into ice-cold water
  3. extractionThe product is extracted
  4. dry with materialThe organic solution is dried over magnesium sulphate
  5. filtrationfollowed by filtration and concentration under vacuum
  6. customPurification
  7. customis then carried out by crystallization from diisopropyl ether
  8. customthe solid obtained
  9. filtrationis filtered
  10. washrinsed with isopentane in order
  11. customto obtain
  12. customafter drying

출처 및 근거

ORD 기록
ord-b1bbe7d7e7304ccbbcef895c9a6e3649
출처 데이터셋
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07285664B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트