Acetic Acid → HCID 13151266、化合物

HRID 344595

反応式

HRID 344595 の反応式
[CH2:1]([O:4][C:5]1[CH:6]=[C:7]([C:9]([F:13])=[CH:10][C:11]=1[Cl:12])[NH2:8])[CH:2]=[CH2:3].[CH2:14]1[CH:19]2[C:20]([O:22][C:23](=O)[CH:18]2[CH2:17][CH:16]=[CH:15]1)=[O:21].C(O)(=O)C>O>[CH2:1]([O:4][C:5]1[CH:6]=[C:7]([N:8]2[C:20](=[O:21])[C:19]3[CH2:14][CH2:15][CH2:16][CH2:17][C:18]=3[C:23]2=[O:22])[C:9]([F:13])=[CH:10][C:11]=1[Cl:12])[CH:2]=[CH2:3]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 6810Tetrahydrophthalic anhydrideHCID 132729264-Chloro-2-fluoro-5-[(prop-2-en-1-yl)oxy]aniline

生成物 1

HCID 13151266HCID 13151266、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A mixture of 9.0 g of 19A, 6.8 g of THPA and 100 mL of glacial acetic acid was heated at reflux temperature for 4 hours. The resulting mixture was cooled to room temperature, poured into 450 mL of water and extracted with ether. The extract phase was washed with water, dried (Na2SO4), and filtered, and the solvent was evaporated from the filtrate. The residue was flash-chromatographed on silica gel, with a 15:85 v:v mixture of ethyl acetate and hexane as eluent, to give N-(3-(allyloxy)-4-chloro-6-fluorophenyl)-3,4,5,6-tetrahydrophthalimide (19B), as an orange oil.

後処理

  1. temperaturewas heated
  2. temperatureat reflux temperature for 4 hours
  3. extractionextracted with ether
  4. washThe extract phase was washed with water
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. customthe solvent was evaporated from the filtrate
  8. customThe residue was flash-chromatographed on silica gel, with a 15:85 v
  9. additionv mixture of ethyl acetate and hexane as eluent

出典と根拠

ORDレコード
ord-c5c913faacfa489ca53cd32ebd138158
出典データセット
uspto-grants-1991_10
特許番号
US05053071

関連ノート

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