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Potassium Carbonate → HCID 66653710, 화합물

HRID 2036200
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HRID 2036200 반응식
[CH2:1]([O:8][C:9]([N:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]1[C:21]1[CH:26]=[C:25]([Cl:27])[CH:24]=[CH:23][C:22]=1[OH:28])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C[O:30][C:31](=[O:45])[C@@H:32](OS(C1C=CC(C)=CC=1)(=O)=O)[CH3:33].C(=O)([O-])[O-].[K+].[K+]>CC#N>[CH2:1]([O:8][C:9]([N:11]1[CH2:20][CH2:19][C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[CH:12]1[C:21]1[CH:26]=[C:25]([Cl:27])[CH:24]=[CH:23][C:22]=1[O:28][C@@H:32]([C:31]([OH:45])=[O:30])[CH3:33])=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1
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참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 12884152Propanoic acid, 2-[[(4-methylphenyl)sulfonyl]oxy]-, methyl ester, (S)-2회HCID 66653819HCID 66653819, 화합물

생성물 1

HCID 66653710HCID 66653710, 화합물

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
65 °C

실험 절차

To a solution of (±)-1-(5-chloro-2-hydroxy-phenyl)-3,4-dihydro-1H-isoquinoline-2-carboxylic acid benzyl ester (192 mg, 0.30 mmol, 1.0 eq.) in MeCN (1 mL), (S)-2-(toluene-4-sulfonyloxy)-propionic acid methyl ester (80 mg, 0.30 mmol, 1.0 eq.) and potassium carbonate anhydrous (83 mg, 0.60 mmol, 2.0 eq.) were added and the mixture was heated to 65° C. for 18 hours. (S)-2-(Toluene-4-sulfonyloxy)-propionic acid methyl ester (40 mg, 0.15 mmol, 0.5 eq.) was added again and the mixture was heated at 90° C. for 4 hours. The mixture was allowed to cool to r.t. and extracted with Et2O (2×), dried over MgSO4, filtered, and concentrated in vacuo. To a solution of the crude ester in THF (1.3 mL), 1M aq. NaOH soln. (0.38 mL) was added. The solution was stirred at r.t. for 18 hours. The solution was diluted with water (2 mL) and 1M aq. HCl soln. (0.38 mL) followed by DCM. The mixture was shaked then the layers were separated and the aq. phase was extracted with DCM (2×). The comb. org. phases were concentrated in vacuo. The crude mixture, redissolved in DMF (1.2 mL), was purified by prep. HPLC (column: Atlantis, 19×50 mm, 5 um, UV/MS, acidic conditions) to give the desired acid.

후처리

  1. temperaturethe mixture was heated at 90° C. for 4 hours
  2. temperatureto cool to r.t.
  3. extractionextracted with Et2O (2×)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo
  7. addition(0.38 mL) was added
  8. additionThe solution was diluted with water (2 mL) and 1M aq. HCl soln
  9. customthe layers were separated
  10. extractionthe aq. phase was extracted with DCM (2×)
  11. concentrationphases were concentrated in vacuo
  12. dissolutionThe crude mixture, redissolved in DMF (1.2 mL)
  13. customwas purified by prep

출처 및 근거

ORD 기록
ord-09794b7f4acd4b3aa379e9971a7b4a7e
출처 데이터셋
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08575158B2

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