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ノート

反応式

HRID 36910 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d92df32fa3c24976935b2b186cc36c14
出典データセット
uspto-grants-1995_05
特許番号
US05418248

反応ノート

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