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

HRID 358098

반응식

HRID 358098 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-85153871b7564d3cbf932dc1559b1ece
출처 데이터셋
uspto-grants-1984_08
특허 번호
US04464382

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