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Potassium Carbonate → tert-butyl 3-(1H-indol-5-yl)-1,2,4-thiadiazol-5-ylcarbamate

HRID 634260
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HRID 634260 반응식
Br[C:2]1[N:6]=[C:5]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11])[S:4][N:3]=1.[NH:15]1[C:23]2[C:18](=[CH:19][C:20](B(O)O)=[CH:21][CH:22]=2)[CH:17]=[CH:16]1.C([O-])([O-])=O.[K+].[K+]>O1CCOCC1.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH:15]1[C:23]2[C:18](=[CH:19][C:20]([C:2]3[N:6]=[C:5]([NH:7][C:8](=[O:14])[O:9][C:10]([CH3:13])([CH3:12])[CH3:11])[S:4][N:3]=3)=[CH:21][CH:22]=2)[CH:17]=[CH:16]1
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반응물 3

HCID 11430Potassium CarbonateHCID 27343615-Indolylboronic acidHCID 44604453tert-Butyl (3-bromo-1,2,4-thiadiazol-5-yl)carbamate

생성물 1

HCID 68356726tert-butyl 3-(1H-indol-5-yl)-1,2,4-thiadiazol-5-ylcarbamate수율 44.2%

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매
HCID 312751,4-Dioxane용매

실험 절차

To a mixture of tert-butyl (3-bromo-1,2,4-thiadiazol-5-yl)carbamate (100 mg, 0.359 mmol) and indole-5-boronic acid (57.9 mg, 0.359 mmol) in 1,4-dioxane (5 mL) was added Pd(PPh3)4 (20.77 mg, 0.017 mmol) and 1M aq K2CO3 solution (0.539 mL, 0.539 mmol). N2 gas was purged for 15 min. After 15 min, the reaction was heated at reflux for 4 h. The reaction mixture was cooled to RT and treated with H2O (5 mL), extracted with EtOAc (25 mL). The aqueous layer was back extracted with EtOAc (25 mL). The combined organic layers were dried over anhydrous Na2SO4 and concentrated. The crude was further purified by silica gel column chromatography (eluent: 10% EtOAc in petroleum ether) to afford tert-butyl (3-(1H-indol-5-yl)-1,2,4-thiadiazol-5-yl)carbamate (50 mg, 44.2%) as an off white solid. MS (ESI, pos. ion) m/z: 261 (M+1); 1H NMR (400 MHz, DMSO-d6): δ 12.40 (s, 1H), 11.31 (s, 1H), 8.35 (s, 1H), 7.91 (dd, J=1.2 Hz & 8.4 Hz, 1H), 7.46 (d, J=8.4 Hz, 1H), 7.41-7.40 (m, 1H), 6.35 (s, 1H), 1.52 (s, 9H).

후처리

  1. customN2 gas was purged for 15 min
  2. temperaturethe reaction was heated
  3. temperatureat reflux for 4 h
  4. additiontreated with H2O (5 mL)
  5. extractionextracted with EtOAc (25 mL)
  6. extractionThe aqueous layer was back extracted with EtOAc (25 mL)
  7. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
  8. concentrationconcentrated
  9. customThe crude was further purified by silica gel column chromatography (eluent: 10% EtOAc in petroleum ether)

출처 및 근거

ORD 기록
ord-4930042288cf4bf7aed8ce4f4f2fb1e9
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321756B2

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