Potassium Carbonate → Toluene-4-thiosulfonic acid S-[3(ethylisopropylamino)-propyl]ester

HRID 707676노트

반응식

HRID 707676 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].[CH2:16]([NH:18][CH:19]([CH3:21])[CH3:20])[CH3:17].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:16]([N:18]([CH:19]([CH3:21])[CH3:20])[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])[CH3:17]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 88318IsopropylethylamineHCID 67607671Toluene-4-thiosulfonic acid S-(3-chloropropyl)ester

생성물 1

HCID 67606220Toluene-4-thiosulfonic acid S-[3(ethylisopropylamino)-propyl]ester

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Toluene-4-thiosulfonic acid S-(3-chloro-propyl) ester (12.0 g, 45.3 mol, 1.00 eq.), N-ethylisopropylamine (4.2 g, 48.0 mmol, 1.05 eq.) and potassium carbonate (6.9 g, 49.9 mmol, 1.10 eq.) were stirred together in acetonitrile (160 mL) at 60° C. for 18 hours. The mixture was concentrated in vacuo and the residue was partitioned between ethyl acetate (500 mL) and water (250 mL). The organic solution was washed with brine (250 mL), dried (MgSO4) and the resulting oil was purified by MPLC chromatography to give an oil weighing 2.98 g (21%).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was partitioned between ethyl acetate (500 mL) and water (250 mL)
  3. washThe organic solution was washed with brine (250 mL)
  4. dry with materialdried (MgSO4)
  5. customthe resulting oil was purified by MPLC chromatography
  6. customto give an oil

출처 및 근거

ORD 기록
ord-795a681f2d07409491848ad636f447b5
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09175042B2

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