Dicyclohexylcarbodiimide → HCID 19816115、化合物

HRID 2247989ノート

反応式

HRID 2247989 の反応式
[SH:1][C:2]1[S:3][CH2:4][CH2:5][N:6]=1.C1(N=C=NC2CCCCC2)CCCCC1.[CH3:22][O:23][CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][CH2:33][C:34](O)=[O:35])=[CH:28][C:27]=1[O:37][CH3:38]>ClCCl.CN(C)C1C=CN=CC=1>[CH3:22][O:23][CH2:24][O:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][CH2:33][C:34]([N:6]2[CH2:5][CH2:4][S:3][C:2]2=[S:1])=[O:35])=[CH:28][C:27]=1[O:37][CH3:38]

参加物

6

反応物 3

HCID 10868DicyclohexylcarbodiimideHCID 19816111HCID 19816111、化合物HCID 178527880HCID 178527880、化合物

生成物 1

HCID 19816115HCID 19816115、化合物

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

In an atmosphere of argon 4.03 g of 3-(4-methoxymethoxy-3-methoxyphenyl)propionic acid and 1.79 g of 2-mercaptothiazoline were dissolved in 80 ml of dichloromethane followed by the addition of 3.10 g of dicyclohexylcarbodiimide and 0.21 g of 4-dimethylaminopyridine. The mixture was stirred at room temperature for 15 hours, and the reaction mixture was filtered. The filtrate was washed with a 1N aqueous sodium hydroxide, water and saturated aqueous sodium chloride and dried over anhydrous magnesium sulfate. The solvent was removed by distillation under reduced pressure, and the residue subjected to column chromatography on silica gel. From the fraction eluted with methylene chloride was obtained 5.07 g of N-[3-(4-methoxymethoxy-3-methoxyphenyl)propanoyl]-thiazolidine-2thione.

後処理

  1. filtrationthe reaction mixture was filtered
  2. washThe filtrate was washed with a 1N aqueous sodium hydroxide, water and saturated aqueous sodium chloride
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under reduced pressure
  5. washFrom the fraction eluted with methylene chloride

出典と根拠

ORDレコード
ord-878a539fb90647c8ae656df29e9c99bb
出典データセット
uspto-grants-1991_08
特許番号
US05037837

反応ノート

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