Water → HCID 21845561、化合物

HRID 619069ノート

反応式

HRID 619069 の反応式
[H-].[Na+].[OH:3][C:4]1[CH:5]=[C:6]([C:14]2[N:15]=[C:16]([NH:19][S:20]([C:23]3[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=3)(=[O:22])=[O:21])[S:17][CH:18]=2)[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[C:9]=1[OH:10].O.[CH3:31]N(C)C=O>>[OH:3][C:4]1[CH:5]=[C:6]([C:14]2[N:15]=[C:16]([NH:19][S:20]([C:23]3[CH:28]=[CH:27][C:26]([CH3:29])=[CH:25][CH:24]=3)(=[O:22])=[O:21])[S:17][CH:18]=2)[CH:7]=[C:8]([N+:11]([O-:13])=[O:12])[C:9]=1[O:10][CH3:31]

参加物

5

反応物 4

HCID 962WaterHCID 6228DimethylformamideHCID 24758Sodium hydrideHCID 21845565HCID 21845565、化合物

生成物 1

HCID 21845561HCID 21845561、化合物

実験手順

50 mg of sodium hydride (60%) were added to a solution of 0.5 g of N-[4-(3,4-dihydroxy-5-nitro-phenyl)-thiazol-2-yl]-4-methyl-benzenesulfonamide in 5 ml of dimethylformamide. The mixture was stirred at room temperature for 1 hour. The reaction mixture was poured into water and extracted with ethyl acetate. The organic phase was dried with magnesium sulphate and concentrated. The residue was chromatographed on 60 g of Kieselgel 60 with methylene chloride/acetone/formic acid (90:10:2.5) as the eluent. The product-containing fractions were concentrated and, after boiling with 20 ml of diethyl ether, yielded 0.17 g of N-[4-(3-hydroxy-4-methoxy-5-nitro-phenyl)-thiazol-2-yl]-4-methyl-benzenesulfonamide as orange colored crystals.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic phase was dried with magnesium sulphate
  3. concentrationconcentrated
  4. customThe residue was chromatographed on 60 g of Kieselgel 60 with methylene chloride/acetone/formic acid (90:10:2.5) as the eluent
  5. concentrationThe product-containing fractions were concentrated

出典と根拠

ORDレコード
ord-7dbf44d9d00048ac941f24bd8d0d2b51
出典データセット
uspto-grants-1999_09
特許番号
US05958910

反応ノート

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