Hydrochloric Acid → 2,4-Thiazolidinedione, 5-((4-((3,4-dihydro-6-hydroxy-5,7,8-trimethyl-2H-1-benzopyran-2-yl)methoxy)phenyl)methyl)-

HRID 1589686ノート

反応式

HRID 1589686 の反応式
C([O:4][C:5]1[C:6]([CH3:33])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][CH:10]([CH2:17][O:18][C:19]1[CH:32]=[CH:31][C:22]([CH2:23][CH:24]3[S:28][C:27](=N)[NH:26][C:25]3=[O:30])=[CH:21][CH:20]=1)[CH2:9][CH2:8]2)(=O)C.Cl.[OH2:35]>COCCO>[OH:4][C:5]1[C:6]([CH3:33])=[C:7]2[C:12](=[C:13]([CH3:16])[C:14]=1[CH3:15])[O:11][CH:10]([CH2:17][O:18][C:19]1[CH:20]=[CH:21][C:22]([CH2:23][CH:24]3[S:28][C:27](=[O:35])[NH:26][C:25]3=[O:30])=[CH:31][CH:32]=1)[CH2:9][CH2:8]2

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 962WaterHCID 140341620HCID 140341620、化合物

生成物 1

HCID 99542592,4-Thiazolidinedione, 5-((4-((3,4-dihydro-6-hydroxy-5,7,8-trimethyl-2H-1-benzopyran-2-yl)methoxy)phenyl)methyl)-

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

実験手順

290 mg of 5-[4-(6-acetoxy-5,7,8-trimethylchroman-2-ylmethoxy)benzyl]-2-iminothiazolidin-4-one (prepared as described in Example 4) were added to a mixture of 3 ml of concentrated hydrochloric acid, 1.5 ml of water and 5 ml of ethylene glycol monomethyl ether, and the mixture was heated under reflux for 3.5 hours. The reaction mixture was then processed and purified as described in Example 1(a), and the crude product, in the form of an oil, was subjected to column chromatography through silica gel. The title compound, melting at 158°-159° C., was obtained from the fractions eluted with a 4:1 by volume mixture of benzene and ethyl acetate.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 3.5 hours
  3. custompurified

出典と根拠

ORDレコード
ord-124afa9d90e14a77bdbdfc17b244932e
出典データセット
uspto-grants-1986_02
特許番号
US04572912

反応ノート

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