Hydrochloric Acid → 5-Oxo-1-(4-sulfophenyl)pyrazolidine-3-carboxylic acid

HRID 839420ノート

反応式

HRID 839420 の反応式
[C:1]([O:8]C)(=[O:7])/[CH:2]=[CH:3]\[C:4]([O-])=[O:5].[NH:10]([C:12]1[CH:17]=[CH:16][C:15]([S:18]([O-:21])(=[O:20])=[O:19])=[CH:14][CH:13]=1)[NH2:11].C(=O)([O-])[O-].[Na+].[Na+].Cl>O>[C:1]([CH:2]1[CH2:3][C:4](=[O:5])[N:10]([C:12]2[CH:17]=[CH:16][C:15]([S:18]([OH:21])(=[O:19])=[O:20])=[CH:14][CH:13]=2)[NH:11]1)([OH:8])=[O:7]

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 10340Sodium Carbonate2 回HCID 1549500p-Hydrazinobenzene sulphonateHCID 21768182Mono-methyl maleate

生成物 1

HCID 203245745-Oxo-1-(4-sulfophenyl)pyrazolidine-3-carboxylic acid収率 85%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

110 parts of monomethyl maleate are added with stirring to 800 parts of water containing 152 parts of p-hydrazinobenzene sulphonate and 88 parts of sodium carbonate. The mixture is warmed until all reactants are in solution and the pH is adjusted by addition of sodium carbonate to 7.0. The resulting solution is heated at 100° C for 9 hours during which period the pH is adjusted to 7.0 after 6 hours. On completion of heating, the pH is adjusted to 3.8 by addition of hydrochloric acid and the 3-carboxy-1-(4'-sulphophenyl)-5-pyrazolidone thus formed is filtered off and dried between 50°-100° C. The actual weight yield is 266 parts of strength 77% (determined by N.M.R.) which represents a yield of 85% theory.

後処理

  1. temperatureThe mixture is warmed until all reactants
  2. temperatureOn completion of heating

出典と根拠

ORDレコード
ord-046cfddd66d842988d0e86b3e26fec6f
出典データセット
uspto-grants-1978_06
特許番号
US04095024

反応ノート

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