碳酸钾 → 海萝胶

HRID 30288

反应方程式

HRID 30288 反应方程式
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]

参与物

6

反应物 3

HCID 11430碳酸钾HCID 12305氯甲酸氯乙酯HCID 1317270457-Methyl-5-(1-phenyl-ethyl)-3b,4,5,6,6a,7-hexahydro-1-thia-5-aza-cyclopenta[alpha]pentalene

产物 2

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

试剂、催化剂与溶剂 1

HCID 887(5BETA,17BETA)-17-羟基-17-(甲基-D3)-2'H-雄甾-2-烯并[3,2-C]吡唑-5'(1'H)-酮溶剂

实验过程

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.

后处理

  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)

来源与证据

ORD记录
ord-85d41e6f25a74b478ea7ed29ef94133e
来源数据集
uspto-grants-2008_09
专利号
US07423056B2

关联笔记

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