Dimethylcarbamoyl Chloride → HCID 54199536, 화합물

HRID 1995642노트

반응식

HRID 1995642 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 54199536HCID 54199536, 화합물수율 85%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-1d05c476222749aba537a954b8fab002
출처 데이터셋
uspto-grants-1983_09
특허 번호
US04405632

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