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Acetic Anhydride → HCID 13066702, 화합물

HRID 1163989
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HRID 1163989 반응식
CO[C:3]1[C:8]([O:9][C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[CH3:16])=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:17][C:18]([OH:20])=[O:19].C(OC(=O)C)(=O)C>I>[C:11]1([CH3:16])[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=1[O:9][C:8]1[C:3]2[O:20][C:18](=[O:19])[CH2:17][C:4]=2[CH:5]=[CH:6][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 7918Acetic AnhydrideHCID 13066676HCID 13066676, 화합물

생성물 1

HCID 13066702HCID 13066702, 화합물수율 73.3%

시약·촉매·용매 1

HCID 24841Hydrogen iodide용매

반응 조건

온도
100 °C

실험 절차

2-[2-Methoxy-3-(o-tolyloxy)phenyl]acetic acid (34.0 g) was added to a mixture of acetic anhydride (50 ml) and 50% aqueous solution of hydrogen iodide (100 ml), and the mixture was refluxed under heating for an hour. The reaction mixture was poured into ice-water (1 l) and extracted with diethyl ether. The extract was washed with aqueous sodium hydrogen sulfite and water (twice) successively, dried over magnesium sulfate and then evaporated. The oily residue (34.0 g) was dissolved in acetic anhydride (50 ml), stirred at 100° C. for 1.5 hours and then evaporated. The crystalline residue (29.0 g) was recrystallized from methanol and diisopropyl ether successively to give colorless crystals of 7-(o-tolyloxy)-2,3-dihydrobenzofuran-2-one (22.0 g). mp 110°-111° C.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for an hour
  3. extractionextracted with diethyl ether
  4. washThe extract was washed with aqueous sodium hydrogen sulfite and water (twice) successively,
  5. dry with materialdried over magnesium sulfate
  6. customevaporated
  7. dissolutionThe oily residue (34.0 g) was dissolved in acetic anhydride (50 ml)
  8. customevaporated
  9. customThe crystalline residue (29.0 g) was recrystallized from methanol and diisopropyl ether successively

출처 및 근거

ORD 기록
ord-6c20e1885d084f3581ab52f59dbe6761
출처 데이터셋
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04367238

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