Potassium Carbonate → Toluene-4-thiosulfonic acid S-[3-(4-methyl-piperazin-1-yl)-propyl]ester

HRID 707677노트

반응식

HRID 707677 반응식
Cl[CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]1[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=1)(=[O:8])=[O:7].[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([CH2:2][CH2:3][CH2:4][S:5][S:6]([C:9]2[CH:14]=[CH:13][C:12]([CH3:15])=[CH:11][CH:10]=2)(=[O:8])=[O:7])[CH2:19][CH2:18]1

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 531671-MethylpiperazineHCID 67607671Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

생성물 1

HCID 67608237Toluene-4-thiosulfonic acid S-[3-(4-methyl-piperazin-1-yl)-propyl]ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Toluene-4-thiosulfonic acid S-(3-chloro-propyl) ester (4.9 g, 18.4 mol, 1.00 eq.), N-methylpiperazine (1.9 g, 19.3 mmol) 1.05 eq.) and potassium carbonate (2.7 g, 19.4 mmol, 1.05 eq.) were stirred together in acetonitrile (100 mL) at room temperature for 64 hours. The mixture was concentrated and the residue was partitioned between ethyl acetate (500 ml) and water (250 ml). The organic solution was washed with water (2×200 mL), dried using MgSO4, concentrated and purified by MPLC to give a light yellow oil weighing 2.1 g (36%).

후처리

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between ethyl acetate (500 ml) and water (250 ml)
  3. washThe organic solution was washed with water (2×200 mL)
  4. customdried
  5. concentrationconcentrated
  6. custompurified by MPLC
  7. customto give a light yellow oil

출처 및 근거

ORD 기록
ord-5e979d64bdb04b50b254a4f59083e782
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175042B2

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