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

HRID 66633

반응식

HRID 66633 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

(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.

후처리

  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°

출처 및 근거

ORD 기록
ord-2c4679b529964aa396a5d7fbf8199685
출처 데이터셋
uspto-grants-1982_08
특허 번호
US04342777

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