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Potassium Carbonate → Methyl 3-{4-[2-(6-benzoyl-2-oxo-1,3-benzothiazol-3(2H)-yl)ethoxy]phenyl}-2-ethoxypropanoate

HRID 1790240
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HRID 1790240 반응식
C(=O)([O-])[O-:2].[K+].[K+].[C:7]([C:15]1[CH:24]=[CH:23][C:18]2[N:19]=[CH:20][S:21](=O)[C:17]=2[CH:16]=1)(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.Cl[CH2:26][CH2:27][O:28][C:29]1[CH:34]=[CH:33][C:32]([CH2:35][CH:36]([O:41][CH2:42][CH3:43])[C:37]([O:39][CH3:40])=[O:38])=[CH:31][CH:30]=1>CN(C)C=O>[C:7]([C:15]1[CH:24]=[CH:23][C:18]2[N:19]([CH2:26][CH2:27][O:28][C:29]3[CH:34]=[CH:33][C:32]([CH2:35][CH:36]([O:41][CH2:42][CH3:43])[C:37]([O:39][CH3:40])=[O:38])=[CH:31][CH:30]=3)[C:20](=[O:2])[S:21][C:17]=2[CH:16]=1)(=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 11616212Methyl 3-[4-(2-chloroethoxy)phenyl]-2-ethoxypropanoateHCID 1317171596-Benzoylbenzothiazolinone

생성물 1

HCID 11584254Methyl 3-{4-[2-(6-benzoyl-2-oxo-1,3-benzothiazol-3(2H)-yl)ethoxy]phenyl}-2-ethoxypropanoate

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
100 °C

실험 절차

To 20 ml of dimethylformamide add potassium carbonate (0.01044 mol) and then 6-benzoylbenzothiazolinone (0.00453 mol). Heat at 100° C. for 1 hour. Add the compound obtained in Step B (0.00348 mol) and heat at 150° C. for 16 hours. Evaporate off the dimethylformamide. Take up the residue in 50 ml of water and then extract with 50 ml of dichloromethane twice. The organic phase is dried over MgSO4 and then evaporated. The residue is recrystallised from methanol and yields the title compound in the form of a solid.

후처리

  1. temperatureheat at 150° C. for 16 hours
  2. customEvaporate off the dimethylformamide
  3. extractionextract with 50 ml of dichloromethane twice
  4. dry with materialThe organic phase is dried over MgSO4
  5. customevaporated
  6. customThe residue is recrystallised from methanol

출처 및 근거

ORD 기록
ord-18b711fee87f4c259f9e62bbac53b196
출처 데이터셋
uspto-grants-2006_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07071221B2

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