Potassium Carbonate → Hydrochloric Acid

HRID 30288

반응식

HRID 30288 반응식
C([O-])([O-])=O.[K+].[K+].[CH3:7][CH:8]1[C:15]2[S:14][CH:13]=[CH:12][C:11]=2[CH:10]2[CH2:16][N:17](C(C3C=CC=CC=3)C)[CH2:18][CH:9]12.[Cl:27]CCOC(Cl)=O>CO>[CH3:7][CH:8]1[C:15]2[S:14][CH:13]=[CH:12][C:11]=2[CH:10]2[CH2:16][NH:17][CH2:18][CH:9]12.[ClH:27]

참가 물질

6

반응물 3

HCID 11430Potassium CarbonateHCID 123052-Chloroethyl chloroformateHCID 1317270457-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene

생성물 2

HCID 313Hydrochloric AcidHCID 597894257-Methyl-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

K2CO3 (320 mg, 2.32 mmol) was added to a solution of the product from step g) (165 mg, 0.58 mmol) in 6 mL followed by the addition of 2-chloroethylchloroformate (332 mg, 2.32 mmol) under vigorous stirring at room temperature. Next, the reaction was stirred for two hours at 75° C. after which the reaction mixture was cooled, filtered and the solvent was evaporated to leave an oily residue that was then dissolved in dry methanol (10 mL) and was stirred at room temperature for one hour. The solvent was evaporated and the residue was triturated in diethyl ether (5 mL) to give the subtitle compound as its HCl salt. MS calculated for C10H13NS+H: 180, observed: 180. 1H NMR (CDCl3300 MHz) δ 1.32 (d, 3H), 1.93 (s, 1H), 3.04 (m, 1H), 3.18 (m, 2H), 3.47 (m, 3H), 3.78 (m, 1H), 6.83 (d, 1H), 7.21 (d, 1H) ppm.

후처리

  1. stirringNext, the reaction was stirred for two hours at 75° C. after which the reaction mixture
  2. temperaturewas cooled
  3. filtrationfiltered
  4. customthe solvent was evaporated
  5. customto leave an oily residue that
  6. stirringwas stirred at room temperature for one hour
  7. customThe solvent was evaporated
  8. customthe residue was triturated in diethyl ether (5 mL)

출처 및 근거

ORD 기록
ord-85d41e6f25a74b478ea7ed29ef94133e
출처 데이터셋
uspto-grants-2008_09
특허 번호
US07423056B2

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