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Triethylamine → Phthalidyl o-acetylsalicylate

HRID 127603
ノート
印刷プレビュー

反応式

HRID 127603 の反応式
[C:1]([C:4]1([OH:13])[CH:12]=[CH:11][CH:10]=[CH:9][CH:5]1[C:6]([OH:8])=[O:7])(=[O:3])[CH3:2].C(N(CC)CC)C.Br[CH:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:24](=[O:25])[O:23]1>CC(C)=O>[C:1]([C:4]1([OH:13])[CH:12]=[CH:11][CH:10]=[CH:9][CH:5]1[C:6]([O:8][CH:22]1[C:31]2[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=2)[C:24](=[O:25])[O:23]1)=[O:7])(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 962181(3H)-Isobenzofuranone, 3-bromo-HCID 178417052-Acetylsalicylic acid

生成物 1

HCID 70571343Phthalidyl o-acetylsalicylate収率 84.4%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

o-Acetylsalicylic acid (18 g) and triethylamine (21 ml) were stirred at a temperature of 20°-25° C. for 30 minutes in 500 ml of acetone. When dissolution was completed, 3-bromophthalide (32 g) was added and the mixture refluxed 2 hours. The reaction mixture was then cooled to 20°-25° C. and poured into distilled water (500 ml). The resulting mixture was extracted with 200 ml of dichloromethane twice, discarding the acetone layer. After the organic solution was washed with 200 ml portions of distilled water twice, 5 g of anhydrous sodium sulfate were added and the mixture filtered. After filtration the organic filtrate was evaporated, the residue was taken up with previously warmed methanol. Decolorizing carbon (1 g) and filtering aid (1 g) were added. The methanolic solution was filtered, and the filtrate was cooled, first to room temperature, and subsequently in an ice/water bath. The solid precipitate was collected by filtration, and dried under vacuum at 40° C. to obtain a yield (83.9%; 26.2 g) of crude phthalidyl o-acetylsalicylate (m.p. 85° C.-88° C.).

後処理

  1. dissolutionWhen dissolution
  2. temperaturethe mixture refluxed 2 hours
  3. temperatureThe reaction mixture was then cooled to 20°-25° C.
  4. additionpoured
  5. distillationinto distilled water (500 ml)
  6. extractionThe resulting mixture was extracted with 200 ml of dichloromethane twice
  7. washAfter the organic solution was washed with 200 ml portions of distilled water twice
  8. addition5 g of anhydrous sodium sulfate were added
  9. filtrationthe mixture filtered
  10. filtrationAfter filtration the organic filtrate
  11. customwas evaporated
  12. filtrationDecolorizing carbon (1 g) and filtering aid (1 g)
  13. additionwere added
  14. filtrationThe methanolic solution was filtered
  15. filtrationThe solid precipitate was collected by filtration
  16. customdried under vacuum at 40° C.
  17. customto obtain

出典と根拠

ORDレコード
ord-6dec7b63204649cea518399874221ad8
出典データセット
uspto-grants-1981_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04256760

反応ノート

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