Potassium Carbonate → Hydrochloric Acid

HRID 30288

反応式

HRID 30288 の反応式
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]

参加物

6

反応物 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

生成物 2

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-85d41e6f25a74b478ea7ed29ef94133e
出典データセット
uspto-grants-2008_09
特許番号
US07423056B2

関連ノート

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