Potassium Carbonate → HCID 86683431, 화합물

HRID 579456노트

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HRID 579456 반응식
Br[C:2]1[S:3][C:4]2[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=2[N:6]=1.Cl.[CH:13]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)([CH3:15])[CH3:14].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH:13]([N:16]1[CH2:21][CH2:20][N:19]([C:2]2[S:3][C:4]3[CH:10]=[C:9]([OH:11])[CH:8]=[CH:7][C:5]=3[N:6]=2)[CH2:18][CH2:17]1)([CH3:15])[CH3:14]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 161884471-Isopropyl-piperazine hydrochlorideHCID 451167822-Bromo-1,3-benzothiazol-6-ol

생성물 1

HCID 86683431HCID 86683431, 화합물수율 18%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

2-Bromo-6-hydroxybenzothiazole (345 mg, 1.5 mmol), 1-isopropyl-piperazine hydrochloride (271 mg, 1.65 mmol) and dry potassium carbonate (828 mg, 6.00 mmol), were dissolved in 6 mL, of dry N,N-dimethylformamide. The resulted pale brown solution was stirred at 100° C. for 18 h in a closed vial. The reaction mixture was evaporated, suspended in 20 mL of water and extracted with dichloromethane (3×15 mL). The combined organic layers were washed with saturated sodium bicarbonate and brine, then dried over MgSO4. After evaporation the residue was purified by column chromatography (Kieselgel 60) using chloroform-methanol 49:1 as the eluent. The title compound (76 mg, 0.27 mmol, 18%) was obtained as a white solid.

후처리

  1. customThe reaction mixture was evaporated
  2. extractionextracted with dichloromethane (3×15 mL)
  3. washThe combined organic layers were washed with saturated sodium bicarbonate and brine
  4. dry with materialdried over MgSO4
  5. customAfter evaporation the residue
  6. customwas purified by column chromatography (Kieselgel 60)

출처 및 근거

ORD 기록
ord-e67e41a5abab4f0da95fb83afa0fbbd4
출처 데이터셋
uspto-grants-2015_05
특허 번호
US09040714B2

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