Dimethylcarbamoyl Chloride → HCID 54199536、化合物

HRID 1995642ノート

反応式

HRID 1995642 の反応式
[H-].[Na+].[CH3:3][C:4]1([CH3:14])[S:8][C:7]2=[N:9][CH:10]=[CH:11][N:6]2[C:5]1=[N:12][OH:13].[CH3:15][N:16]([CH3:20])[C:17](Cl)=[O:18]>O1CCCC1>[CH3:3][C:4]1([CH3:14])[S:8][C:7]2=[N:9][CH:10]=[CH:11][N:6]2[C:5]1=[N:12][O:13][C:17](=[O:18])[N:16]([CH3:20])[CH3:15]

参加物

5

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 24758Sodium hydrideHCID 71420982N-(2,2-Dimethylimidazo[2,1-b][1,3]thiazol-3(2H)-ylidene)hydroxylamine

生成物 1

HCID 54199536HCID 54199536、化合物収率 85%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 330 mg (13.6 mmol) of sodium hydride in 150 ml of dry tetrahydrofuran was added 2.50 g (13.6 mmol) of 2,2-dimethyl-3-hydroxyimino-2,3-dihydroimidazo-[2,1-b]thiazole. The reaction mixture was stirred at 25° for 1 hour and cooled in an ice bath before 1.54 g (14.3 mmol) of dimethylcarbamoyl chloride was added. After stirring for 12 hours at 25°, the solvent was removed in vacuo and the residue washed with hexane, dissolved in methylene chloride. The methylene chloride solution was washed with water, dried (MgSO4), and concentrated in vacuo to give 2.94 g (85%) of desired product. m.p. 99°-102.5°.

後処理

  1. additionwas added
  2. stirringAfter stirring for 12 hours at 25°
  3. customthe solvent was removed in vacuo
  4. washthe residue washed with hexane
  5. dissolutiondissolved in methylene chloride
  6. washThe methylene chloride solution was washed with water
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1d05c476222749aba537a954b8fab002
出典データセット
uspto-grants-1983_09
特許番号
US04405632

反応ノート

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