Methanol → (E,E)-3-Carboxymethyl-5-(2-methylcinnamylidene)rhodanine N-methyl-D-glucamine salt

HRID 358098

反応式

HRID 358098 の反応式
[CH3:1][NH:2][CH2:3][C@@H:4]([C@H:6]([C@@H:8]([C@@H:10]([CH2:12][OH:13])[OH:11])[OH:9])[OH:7])[OH:5].[C:14]([CH2:17][N:18]1[C:22](=[O:23])[C:21](=[CH:24][CH:25]=[CH:26][C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[CH3:33])[S:20][C:19]1=[S:34])([OH:16])=[O:15].S1CC(=O)NC1=S.CO>O>[CH3:1][NH:2][CH2:3][C@@H:4]([C@H:6]([C@@H:8]([C@@H:10]([CH2:12][OH:13])[OH:11])[OH:9])[OH:7])[OH:5].[C:14]([CH2:17][N:18]1[C:22](=[O:23])/[C:21](=[CH:24]\[CH:25]=[CH:26]\[C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][C:28]=2[CH3:33])/[S:20][C:19]1=[S:34])([OH:16])=[O:15]

参加物

6

反応物 4

HCID 887MethanolHCID 8567N-Methyl-D-glucamineHCID 1201546RhodanineHCID 566395213-Carboxymethyl-5-(2-methylcinnamylidene)rhodanine

生成物 1

HCID 86739588(E,E)-3-Carboxymethyl-5-(2-methylcinnamylidene)rhodanine N-methyl-D-glucamine salt収率 72.5%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

To a solution of 2.001 g of N-methyl-D-glucamine in 20 ml of water was added 3.194 g of 3-carboxymethyl-5-(2-methylcinnamylidene)rhodanine [prepared as described in Example 1 (35)], and the mixture was heated to dissolve the rhodanine derivative, and then 40 ml of methanol was added to the solution at the same temperature. The mixture was cooled to room temperature and the precipitated crystals were filtered. The resulting crystals were washed with 5 ml of mixture of water and methanol (1:2), and 5 ml of methanol, and dried under reduced pressure to obtain 3.73 g of the titled compound.

後処理

  1. temperaturethe mixture was heated
  2. filtrationthe precipitated crystals were filtered
  3. washThe resulting crystals were washed with 5 ml of mixture of water and methanol (1:2), and 5 ml of methanol
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-85153871b7564d3cbf932dc1559b1ece
出典データセット
uspto-grants-1984_08
特許番号
US04464382

関連ノート

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