Water → 4-[[2-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene

HRID 427278노트

반응식

HRID 427278 반응식
[C:1]([NH2:10])(=[O:9])[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].O=[C:12]([CH3:24])[CH2:13][O:14][C:15]1[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=1.N1CCCCC1.O>C1C=CC=CC=1>[CH3:24][C:12]1([CH2:13][O:14][C:15]2[CH:20]=[CH:19][C:18]([N+:21]([O-:23])=[O:22])=[CH:17][CH:16]=2)[NH:10][C:1](=[O:9])[C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4]1

참가 물질

6

반응물 4

HCID 962Water2회HCID 5147SalicylamideHCID 8082PiperidineHCID 3085071-(4-Nitrophenoxy)propan-2-one

생성물 1

HCID 183569464-[[2-Methyl-4-oxo-3,4-dihydro-(2H)-1,3-benzoxazine-2-yl]methoxy]nitrobenzene수율 86%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a stirred mixture of salicylamide (6.85 g, 50 mmol) and 4-[2-oxo-propoxy]nitrobenzene (9.75 g, 50 mmol) in benzene (500 mL) was added piperidine (0.52 mL, 5 mmol). The reaction mixture was immersed in a pre-heated oil bath (˜100° C.) and refluxed for 10 h with continuous removal of water using Dean-Stark water separator. The reaction mixture was cooled to room temperature End the precipitated brown coloured solid was filtered, washed with benzene and dried to afford the title compound (13.5 g, 86%).

후처리

  1. customThe reaction mixture was immersed in a pre-heated oil bath
  2. filtrationwas filtered
  3. washwashed with benzene
  4. customdried

출처 및 근거

ORD 기록
ord-3d08c324cdf244e9b7acf322362868dc
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313113B1

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