Ammonia → 2-oxo-2H-1-benzopyran-7-yl 4-hydroxybenzoate

HRID 2120515ノート

反応式

HRID 2120515 の反応式
N.COC([O:6][C:7]1[CH:26]=[CH:25][C:10]([C:11]([O:13][C:14]2[CH:24]=[CH:23][C:17]3[CH:18]=[CH:19][C:20](=[O:22])[O:21][C:16]=3[CH:15]=2)=[O:12])=[CH:9][CH:8]=1)=O>C(O)C>[OH:6][C:7]1[CH:8]=[CH:9][C:10]([C:11]([O:13][C:14]2[CH:24]=[CH:23][C:17]3[CH:18]=[CH:19][C:20](=[O:22])[O:21][C:16]=3[CH:15]=2)=[O:12])=[CH:25][CH:26]=1

参加物

4

反応物 2

HCID 222AmmoniaHCID 234351152-oxo-2H-1-benzopyran-7-yl 4-methoxycarbonyloxybenzoate

生成物 1

HCID 234351162-oxo-2H-1-benzopyran-7-yl 4-hydroxybenzoate収率 93.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

50 ml of saturated ethanolic ammonia solution is added dropwise to a solution of 12.2 g of 2-oxo-2H-1-benzopyran-7-yl 4-methoxycarbonyloxybenzoate in 200 ml of ethanol. The reaction mixture is stirred for two hours, evaporated down and taken up in 100 ml diethyl ether. This solution is washed with water, dried, filtered to remove inorganic material and the filtrate evaporated down. The residue is purified by column chromatography on silica gel using hexane/ethyl acetate (1/1 v/v) as eluent and recrystallisation from acetonitrile to yield 9.5 g of 2-oxo-2H-1-benzopyran-7-yl 4-hydroxybenzoate.

後処理

  1. customevaporated down
  2. washThis solution is washed with water
  3. customdried
  4. filtrationfiltered
  5. customto remove inorganic material
  6. customthe filtrate evaporated down
  7. customThe residue is purified by column chromatography on silica gel
  8. customrecrystallisation from acetonitrile

出典と根拠

ORDレコード
ord-99d7cfcd4db34573b14dfbcc349b24ea
出典データセット
uspto-grants-2004_02
特許番号
US06692797B1

反応ノート

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