Morpholine → 4-(2,6-Difluoro-4-nitrophenyl)morpholine

HRID 56297노트

반응식

HRID 56297 반응식
[F:1][C:2]1[CH:7]=[C:6]([N+:8]([O-:10])=[O:9])[CH:5]=[C:4]([F:11])[C:3]=1F.[NH:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1.CCN(CC)CC>CCOC(C)=O>[F:11][C:4]1[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=[C:2]([F:1])[C:3]=1[N:13]1[CH2:18][CH2:17][O:16][CH2:15][CH2:14]1

참가 물질

5

반응물 3

HCID 8083MorpholineHCID 8471TriethylamineHCID 27827931,2,3-Trifluoro-5-nitrobenzene

생성물 1

HCID 223856304-(2,6-Difluoro-4-nitrophenyl)morpholine수율 98%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 1,2,3-trifluoro-5-nitrobenzene (3.54 g, 20.0 mmol), morpholine (2.0 mL, 23.0 mmol) and Et3N (8.5 mL, 61.0 mmol) in EtOAc (30 mL) was stirred at rt for 5 h. The mixture was concentrated in vacuo, and the residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1) to give the title compound as a yellow solid (4.76 g, 98%).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was purified by a silica gel column chromatography (PE/EtOAc (V/V)=8:1)

출처 및 근거

ORD 기록
ord-04fd99919e6944dd9f0003da4c38a39a
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434695B2

반응 노트

불러오는 중…