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

HRID 236254
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HRID 236254 반응식
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]
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참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ec12ae60b06b41c0803eb80d956fb700
출처 데이터셋
uspto-grants-1987_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04643849

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