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Sodium Hydroxide → 5-(Dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene

HRID 892788
ノート
印刷プレビュー

反応式

HRID 892788 の反応式
Cl.Cl.C([S:6][CH2:7][C:8]1[S:9][C:10]([CH2:14][N:15]([CH3:17])[CH3:16])=[C:11]([CH3:13])[CH:12]=1)(=N)N.[OH-].[Na+]>O>[CH3:17][N:15]([CH2:14][C:10]1[S:9][C:8]([CH2:7][SH:6])=[CH:12][C:11]=1[CH3:13])[CH3:16]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 138252712-Amidinothiomethyl-5-(dimethylamino)methyl-4-methylthiophene dihydrochloride

生成物 1

HCID 138252725-(Dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene収率 83.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In 5 ml of water was dissolved 10 g of 2-amidinothiomethyl-5-(dimethylamino)methyl-4-methylthiophene dihydrochloride, and 2.52 g of sodium hydroxide was added thereto, and the resulting mixture was subjected to reaction under reflux for 2.5 hours in a nitrogen atmosphere. The reaction mixture was cooled to room temperature, and then extracted with 100 ml of methylene chloride, and the extract was dried over anhydrous magnesium sulfate, after which the solvent was removed by distillation under reduced pressure. The oily substance thus obtained was distilled under reduced pressure in a nitrogen atmosphere to obtain 5.3 g (yield 83%) of 5-(dimethylamino)methyl-2-mercaptomethyl-4-methylthiophene having a boiling point of 102°-105° C./3 mmHg.

後処理

  1. additionwas added
  2. customthe resulting mixture was subjected to reaction
  3. temperatureunder reflux for 2.5 hours in a nitrogen atmosphere
  4. extractionextracted with 100 ml of methylene chloride
  5. dry with materialthe extract was dried over anhydrous magnesium sulfate
  6. customafter which the solvent was removed by distillation under reduced pressure
  7. customThe oily substance thus obtained
  8. distillationwas distilled under reduced pressure in a nitrogen atmosphere

出典と根拠

ORDレコード
ord-9f35b51cd98a4f30acf7b555f04a38b0
出典データセット
uspto-grants-1992_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05120746

反応ノート

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