Acetic Acid → 2,3-Dihydro-2,4-dimethyl-7-nitrobenzofuran

HRID 465020노트

반응식

HRID 465020 반응식
[CH2:1]([C:4]1[C:9]([CH3:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:5]=1[OH:14])[CH:2]=[CH2:3].C(O)(=O)C.Br>CCOCC>[CH3:3][CH:2]1[CH2:1][C:4]2[C:9]([CH3:10])=[CH:8][CH:7]=[C:6]([N+:11]([O-:13])=[O:12])[C:5]=2[O:14]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 260Hydrogen BromideHCID 135756673-Methyl-6-nitro-2-(prop-2-en-1-yl)phenol

생성물 1

HCID 135756682,3-Dihydro-2,4-dimethyl-7-nitrobenzofuran

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

47 g of 1B was added to a mixture of 100 ml of glacial acetic acid and 100 ml of 48% aqueous hydrobromic acid and the mixture was heated at 114°-115° C. for 2.5 hours. The resulting mixture was stripped to dryness, the residue was taken up in 500 ml of ether, and filtered. The filtrate was concentrated to 100 ml, 300 ml of hexane was added, the mixture was chilled and filtered to give 2,3-dihydro-2,4-dimethyl-7-nitrobenzofuran (1C), as a tan solid, m.p.: 69°-71° C.

후처리

  1. temperaturethe mixture was heated at 114°-115° C. for 2.5 hours
  2. filtrationfiltered
  3. concentrationThe filtrate was concentrated to 100 ml, 300 ml of hexane
  4. additionwas added
  5. temperaturethe mixture was chilled
  6. filtrationfiltered

출처 및 근거

ORD 기록
ord-3a1f375c2fda48648d0a751e5ff7d975
출처 데이터셋
uspto-grants-1985_10
특허 번호
US04550121

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