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Citric Acid → 5-methyl-2-{7-[methyl(2-thienylsulfonyl)amino]-1H-indol-2-yl)-4,5-dihydro-1,3-thiazole-5-carboxylic acid

HRID 504688
ノート
印刷プレビュー

反応式

HRID 504688 の反応式
C(C1(C)[S:7][C:6]([C:8]2[NH:9][C:10]3[C:15]([CH:16]=2)=[CH:14][CH:13]=[CH:12][C:11]=3[N:17]([CH3:26])[S:18]([C:21]2[S:22][CH:23]=[CH:24][CH:25]=2)(=[O:20])=[O:19])=[N:5]C1)#N.[OH-].[Na+].O1CCCC1.C(O)(=O)[CH2:36][C:37]([CH2:42]C(O)=O)([C:39]([OH:41])=[O:40])O>C(O)C>[CH3:42][C:37]1([C:39]([OH:41])=[O:40])[S:7][C:6]([C:8]2[NH:9][C:10]3[C:15]([CH:16]=2)=[CH:14][CH:13]=[CH:12][C:11]=3[N:17]([CH3:26])[S:18]([C:21]2[S:22][CH:23]=[CH:24][CH:25]=2)(=[O:20])=[O:19])=[N:5][CH2:36]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 311Citric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 59135902N-[2-(5-cyano-5-methyl-4,5-dihydro-1,3-thiazol-2-yl)-1H-indol-7-yl]-N-methylthiophene-2-sulfonamide

生成物 1

HCID 574761205-methyl-2-{7-[methyl(2-thienylsulfonyl)amino]-1H-indol-2-yl)-4,5-dihydro-1,3-thiazole-5-carboxylic acid収率 69%

試薬・触媒・溶媒

1
HCID 702Ethanol溶媒

実験手順

A mixture of N-[2-(5-cyano-5-methyl-4,5-dihydro-1,3-thiazol-2-yl)-1H-indol-7-yl]-N-methylthiophene-2-sulfonamide (0.15 g), 2N aqueous sodium hydroxide solution (0.36 ml), tetrahydrofuran (3 ml) and ethanol (3 ml) was heated under reflux for 4 hr. 10% Aqueous citric acid solution was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO4), and concentrated. The residue was subjected to silica gel column chromatography to give the title compound (0.11 g, yield 69%) as yellow crystals from a fraction eluted with tetrahydrofuran. melting point >232° C. (decomposition).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 4 hr
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated

出典と根拠

ORDレコード
ord-867ffda24c014b98b8e3c462a266f6f5
出典データセット
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07777047B2

反応ノート

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