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Acetic Anhydride → HCID 13066702、化合物

HRID 1163989
ノート
印刷プレビュー

反応式

HRID 1163989 の反応式
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
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7918Acetic AnhydrideHCID 13066676HCID 13066676、化合物

生成物 1

HCID 13066702HCID 13066702、化合物収率 73.3%

試薬・触媒・溶媒 1

HCID 24841Hydrogen iodide溶媒

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6c20e1885d084f3581ab52f59dbe6761
出典データセット
uspto-grants-1983_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04367238

反応ノート

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