Acetic Acid → 5-Methoxy-6-(2-phenylpropan-2-yl)-1,3-benzodioxole

HRID 66633

反応式

HRID 66633 の反応式
[CH2:1]1[O:5][C:4]2[CH:6]=[C:7]([OH:10])[CH:8]=[CH:9][C:3]=2[O:2]1.[CH3:11][C:12](O)([CH3:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.[C:21](O)(=O)C(O)=O.C(O)(=O)C>O>[CH3:11][C:12]([C:8]1[C:7]([O:10][CH3:21])=[CH:6][C:4]2[O:5][CH2:1][O:2][C:3]=2[CH:9]=1)([CH3:19])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

参加物

6

反応物 4

HCID 176Acetic AcidHCID 971Oxalic AcidHCID 120532-Phenyl-2-propanolHCID 68289Sesamol

生成物 1

HCID 3363345-Methoxy-6-(2-phenylpropan-2-yl)-1,3-benzodioxole

試薬・触媒・溶媒 1

HCID 962Water溶媒2 回

実験手順

(α,α-Dimethylbenzyl)-3,4-methylenedioxy-6-methoxybenzene was prepared as follows: A mixture of sesamol (44 g), α,α-dimethylbenzyl alcohol (44 g), oxalic acid (3 g), acetic acid (100 ml) and water (10 ml) was refluxed for 2.5 hours, diluted with water and extracted with chloroform. Distillation of the chloroform extract gave an oil, b.p. 160°-163° at 0.5 mm Hg (60 g) which crystallized from aqueous methanol to give colorless needles, m.p. 75°-76°; (Found: C, 75.0; H, 6.26. Calc. for C16H16O3 : C, 75.0; H, 6.29%); pmr spectrum: δ1.63, 6H, S; 4.12, 1H, S; δ5.81, 2H, S; δ6.33, 1H, S; δ6.98, 1H, S; δ6.31, 5H, S.

後処理

  1. temperaturewas refluxed for 2.5 hours
  2. extractionextracted with chloroform
  3. distillationDistillation of the chloroform
  4. extractionextract
  5. customgave an oil, b.p. 160°-163° at 0.5 mm Hg (60 g) which
  6. customcrystallized from aqueous methanol
  7. customto give colorless needles, m.p. 75°-76°

出典と根拠

ORDレコード
ord-2c4679b529964aa396a5d7fbf8199685
出典データセット
uspto-grants-1982_08
特許番号
US04342777

関連ノート

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