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

HRID 279890ノート

反応式

HRID 279890 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-322d2b48fe654f38ab93095f0d344369
出典データセット
uspto-grants-1986_05
特許番号
US04587259

反応ノート

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