1-Methylpiperazine → HCID 15557283, compound

HRID 1095533Notes

Reaction equation

HRID 1095533 reaction equation
Br[CH2:2][CH2:3][C:4]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=2)[NH:6][CH:5]=1.[CH3:13][N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>C(Cl)(Cl)Cl>[CH3:13][N:14]1[CH2:19][CH2:18][N:17]([CH2:2][CH2:3][C:4]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[NH:6][CH:5]=2)[CH2:16][CH2:15]1

Participants

4

Conditions

Temperature
75 °C

Procedure

3-(2-Bromo-ethyl)-indole (3.00 g, 13.39 mmol) was initially introduced into abs. CHCl3 (25 ml), and 1-methylpiperazine (2.68 g, 26.8 mmol) was added. The mixture was stirred at a bath temperature of 75° C. for 5 h and at RT overnight. The mixture was extracted dilute sulfuric acid (2×30 ml), the acidic aqueous phase was rendered alkaline with 5N NaOH, while cooling with ice, and the mixture was extracted with ether (3×30 ml). The organic phase was dried over Na2SO4 and concentrated i. vac. Yield: 1.45 g (Ind-68, 45%)

Workup

  1. customat RT
  2. customovernight
  3. extractionThe mixture was extracted dilute sulfuric acid (2×30 ml)
  4. temperaturewhile cooling with ice
  5. extractionthe mixture was extracted with ether (3×30 ml)
  6. dry with materialThe organic phase was dried over Na2SO4
  7. concentrationconcentrated i

Sources & evidence

ORD record
ord-c96199b1726b47caa481c6063d9e117e
Source dataset
uspto-grants-2012_03
Patent number
US08138187B2

Reaction notes

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