4-Toluenesulfonyl chloride → 3-(4-Methyl-piperazin-1-yl)propyl-4-toluene sulphonate

HRID 22770

반응식

HRID 22770 반응식
[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7](Cl)(=[O:9])=[O:8])=[CH:3][CH:2]=1.[OH:12][CH2:13][CH2:14][CH2:15][N:16]1[CH2:21][CH2:20][N:19]([CH3:22])[CH2:18][CH2:17]1.C(N(CC)CC)C>C(Cl)Cl>[C:1]1([CH3:11])[CH:6]=[CH:5][C:4]([S:7]([O:12][CH2:13][CH2:14][CH2:15][N:16]2[CH2:17][CH2:18][N:19]([CH3:22])[CH2:20][CH2:21]2)(=[O:9])=[O:8])=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 73974-Toluenesulfonyl chlorideHCID 8471TriethylamineHCID 792083-(4-Methyl-1-piperazine)propan-1-ol

생성물 1

HCID 218748183-(4-Methyl-piperazin-1-yl)propyl-4-toluene sulphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

4-Toluenesulphonyl chloride (3.2 g) was added to a stirred mixture of 1-(3-hydroxypropyl)-4-methylpiperazine (2.4 g), triethylamine (4.6 ml) and methylene chloride (60 ml) and the resultant mixture was stirred at ambient temperature for 2 hours. The solution was washed in turn with a saturated aqueous sodium bicarbonate solution and with water and filtered through phase separating paper. The organic filtrate was evaporated to give 3-(4-methylpiperazin-1-yl)propyl 4-toluenesulphonate as an oil which crystallised on standing (3.7 g); Mass Spectrum: M+H+ 313.

후처리

  1. washThe solution was washed in turn with a saturated aqueous sodium bicarbonate solution and with water
  2. filtrationfiltered through phase
  3. customseparating paper
  4. customThe organic filtrate was evaporated

출처 및 근거

ORD 기록
ord-3adbcf36c6d84233a6b17dbfbaadf784
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06849625B2

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