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

HRID 1654651

반응식

HRID 1654651 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
150 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9da7c15d4f60414cb0fe0f894f7314bb
출처 데이터셋
uspto-grants-1995_04
특허 번호
US05409919

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