Phthalic Anhydride → 7-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)heptanoic acid

HRID 224980

反応式

HRID 224980 の反応式
[C:1]1(=[O:11])[O:6][C:4](=O)[C:3]2=[CH:7][CH:8]=[CH:9][CH:10]=[C:2]12.[NH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=[O:20]>C(OCC)(=O)C>[C:4]1(=[O:6])[N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][C:19]([OH:21])=[O:20])[C:1](=[O:11])[C:2]2=[CH:10][CH:9]=[CH:8][CH:7]=[C:3]12

参加物

4

反応物 2

HCID 6811Phthalic AnhydrideHCID 135807-Aminoheptanoic acid

生成物 1

HCID 136226357-(1,3-Dioxo-1,3-dihydro-2H-isoindol-2-yl)heptanoic acid収率 50.8%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of phthalic anhydride (5.3 g.) and 7-amino-heptanoic acid (5.8 g.) was heated at 185°-190° C. for 40 minutes and then cooled. The cooled partially solidified product was dissolved in ethyl acetate and the solution washed several times with dilute HCl. The organic layer was dried (MgSO4), filtered and evaporated to dryness and the residue recrystallized from acetic acid to give 7-phthalimidoheptanoic acid (5 g.), m.p. 112°-115° C.

後処理

  1. temperaturewas heated at 185°-190° C. for 40 minutes
  2. temperaturecooled
  3. temperatureThe cooled partially solidified product
  4. washthe solution washed several times with dilute HCl
  5. dry with materialThe organic layer was dried (MgSO4)
  6. filtrationfiltered
  7. customevaporated to dryness
  8. customthe residue recrystallized from acetic acid

出典と根拠

ORDレコード
ord-69f78c92517845a3a70f96df5c84e7fd
出典データセット
uspto-grants-1980_11
特許番号
US04234735

関連ノート

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