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

HRID 2120515노트

반응식

HRID 2120515 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-99d7cfcd4db34573b14dfbcc349b24ea
출처 데이터셋
uspto-grants-2004_02
특허 번호
US06692797B1

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