Captamine → 2-[(Imidazo[1,2-b]pyridazin-6-yl)sulfanyl]-N,N-dimethylethan-1-amine

HRID 1088244

反応式

HRID 1088244 の反応式
[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][SH:5].C[O-].[Na+].Cl[C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[N:16]=1>CO>[CH3:1][N:2]([CH3:6])[CH2:3][CH2:4][S:5][C:11]1[CH:12]=[CH:13][C:14]2[N:15]([CH:17]=[CH:18][N:19]=2)[N:16]=1

参加物

5

反応物 3

HCID 25799CaptamineHCID 138828Imidazo(1,2-b)pyridazine, 6-chloro-HCID 10942334Sodium Methoxide

生成物 1

HCID 200765592-[(Imidazo[1,2-b]pyridazin-6-yl)sulfanyl]-N,N-dimethylethan-1-amine収率 57.6%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
150 °C

実験手順

To 20 ml of methanol is dissolved 2.8 g of 2-dimethylaminoethanethiol. To this, 20 ml of 2M solution of sodium methoxide in methanol and 3 g of 6-chloroimidazo-[1,2-b]pyridazine are added successively and the mixture is heated in a sealed tube for 4 hours at 150° C. After cooling, the solvent is evaporated and the residue is treated with water. The mixture is then extracted with methylene chloride. The organic layer is separated, washed with saturated aqueous solution of sodium chloride and dried over MgSO4. Evaporation of the solvent gives 2.5 g of the title compound as pale yellow crystals.

後処理

  1. temperatureAfter cooling
  2. customthe solvent is evaporated
  3. additionthe residue is treated with water
  4. extractionThe mixture is then extracted with methylene chloride
  5. customThe organic layer is separated
  6. washwashed with saturated aqueous solution of sodium chloride
  7. dry with materialdried over MgSO4
  8. customEvaporation of the solvent

出典と根拠

ORDレコード
ord-6909fea74f704337a14f55ca9286f037
出典データセット
uspto-grants-1990_10
特許番号
US04962100

関連ノート

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