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

Isopropylamine → N-Isopropyl-2-nitroaniline

HRID 334731
노트
인쇄 미리보기

반응식

HRID 334731 반응식
F[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH:11]([NH2:14])([CH3:13])[CH3:12]>CCO>[CH:11]([NH:14][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])([CH3:13])[CH3:12]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6363Isopropylamine3회HCID 738951-Fluoro-2-nitrobenzene

생성물 1

HCID 10583518N-Isopropyl-2-nitroaniline수율 93.1%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of 1-fluoro-2-nitrobenzene (4.406 g, 31.22 mmol) in EtOH (32 mL) was added at 0° C. isopropyl amine (2.97 mL, 32.80 mmol). The mixture turned from light yellow to bright orange instantly. It was stirred overnight at RT. Another 1 eq of isopropyl amine (2.97 mL, 32.80 mmol) was added and after 3 h of stirring 2 eq of isopropyl amine were added (6 mL, 64 mmol) and the resulting solution was kept at room temperature overnight. The reaction mixture was concentrated and another equivalent of isopropyl amine was added (2.97 mL) following by EtOH (2 mL). For completion, the reaction was heated at 50° C. for 2 h. Mixture was evaporated to dryness and dissolved in EtOAc (25 mL) and the organic phase was washed with water (3*10 mL). Aqueous phase was re-extracted with EtOAc (10 mL) and the combined organics were washed with brine and dried over Na2SO4. The solvent was evaporated under reduced pressure to afford 5.24 g of N-isopropyl-2-nitrobenzenamine (Yield: 93%) as an orange liquid

후처리

  1. additionwere added (6 mL, 64 mmol)
  2. waitthe resulting solution was kept at room temperature overnight
  3. concentrationThe reaction mixture was concentrated
  4. additionanother equivalent of isopropyl amine was added (2.97 mL)
  5. temperatureFor completion, the reaction was heated at 50° C. for 2 h
  6. customMixture was evaporated to dryness
  7. dissolutiondissolved in EtOAc (25 mL)
  8. washthe organic phase was washed with water (3*10 mL)
  9. extractionAqueous phase was re-extracted with EtOAc (10 mL)
  10. washthe combined organics were washed with brine
  11. dry with materialdried over Na2SO4
  12. customThe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-83bee91e214d43628566341074a18795
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883826B2

반응 노트

불러오는 중…

이 페이지에서참가 물질실험 절차후처리출처 및 근거반응 노트