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Sulfuric acid magnesium salt (1:1) → (2S)-N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-(4-formylthiazol-2-ylthio)acetamide

HRID 545117
ノート
印刷プレビュー

反応式

HRID 545117 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[CH2:5][N:6]1[CH2:11][CH2:10][O:9][C@@H:8]([CH2:12][NH:13][C:14](=[O:24])[CH2:15][S:16][C:17]2[S:18][CH:19]=[C:20]([CH2:22][OH:23])[N:21]=2)[CH2:7]1.S([O-])([O-])(=O)=O.[Mg+2]>C(Cl)(Cl)Cl.[O-2].[O-2].[Mn+4]>[Cl:1][C:2]1[CH:3]=[C:4]([CH:25]=[CH:26][C:27]=1[Cl:28])[CH2:5][N:6]1[CH2:11][CH2:10][O:9][C@@H:8]([CH2:12][NH:13][C:14](=[O:24])[CH2:15][S:16][C:17]2[S:18][CH:19]=[C:20]([CH:22]=[O:23])[N:21]=2)[CH2:7]1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 24083Sulfuric acid magnesium salt (1:1)2 回HCID 67169032(2S)-N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-[4-(hydroxymethyl)thiazol-2-ylthio]acetamide

生成物 1

HCID 86616376(2S)-N-{[4-(3,4-dichlorobenzyl)morpholin-2-yl]methyl}-(4-formylthiazol-2-ylthio)acetamide

試薬・触媒・溶媒 2

HCID 178418406HCID 178418406、化合物触媒2 回
HCID 6212
Chloroform
溶媒

実験手順

The resultant product (1.53 g) of (70-1) was dissolved in chloroform (10 mL), magnesium sulfate (500 mg) was added, manganese dioxide (1.35 g) was further added, and the mixture was stirred overnight at room temperature. Magnesium sulfate (500 mg) and manganese dioxide (1.35 g) were further added and the mixture was stirred at room temperature for 7 hrs. The reaction mixture was filtered through celite, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography using a mixed solvent of chloroform and methanol as an eluent. The solvent was evaporated from the eluent to give the title compound (643 mg) as a colorless oil.

後処理

  1. stirringthe mixture was stirred at room temperature for 7 hrs
  2. filtrationThe reaction mixture was filtered through celite
  3. customthe solvent was evaporated under reduced pressure
  4. customThe obtained residue was purified by silica gel column chromatography
  5. customThe solvent was evaporated from the eluent

出典と根拠

ORDレコード
ord-0be846eb0e0e405da4a9664bff148cc4
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935700B2

反応ノート

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