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alpha-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride → N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide

HRID 36910
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HRID 36910 반응식
Cl.Cl[CH:3]([C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27])[C:4]([N:6]([CH3:8])[CH3:7])=[O:5].C(S([O-])=O)O.[Na+]>ClCCl>[CH3:8][N:6]([CH3:7])[C:4](=[O:5])[CH2:3][C:9]1[N:16]2[C:12]([S:13][C:14]3[CH:20]=[CH:19][CH:18]=[CH:17][C:15]=32)=[N:11][C:10]=1[C:21]1[CH:25]=[C:24]([CH3:26])[S:23][C:22]=1[CH3:27]
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참가 물질

4

반응물 2

HCID 19936712alpha-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochlorideHCID 23689980Sodium Formaldehyde Sulfoxylate

생성물 1

HCID 19936717N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

34 g (0.077 mole) of α-chloro-N,N-dimethyl-2-(2,5-dimethylthien-3-yl)imidazo[2,1-b]benzothiazole-3-acetamide hydrochloride in solution in 500 ml of dichloromethane are treated with 36.9 g (0.24 mole) of Rongalite®, while stirring the mixture at room temperature for 24 h. The organic phase is separated after settling has taken place, the solid residue is washed with dichloromethane, the organic phase is washed with a saturated sodium hydrogen carbonate solution and then with water, it is dried over sodium sulphate, the solvent is evaporated under reduced pressure and 22 g of solid are obtained. After recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals are finally obtained. Melting point: 194°-195° C.

후처리

  1. customThe organic phase is separated after settling
  2. washthe solid residue is washed with dichloromethane
  3. washthe organic phase is washed with a saturated sodium hydrogen carbonate solution
  4. dry with materialwith water, it is dried over sodium sulphate
  5. customthe solvent is evaporated under reduced pressure and 22 g of solid
  6. customare obtained
  7. customAfter recrystallization from ethanol and treatment with vegetable black, 17 g of pale yellow crystals
  8. customare finally obtained

출처 및 근거

ORD 기록
ord-d92df32fa3c24976935b2b186cc36c14
출처 데이터셋
uspto-grants-1995_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05418248

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