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Chloromethyl Methyl Ether → methyl 5-(4-chlorophenyl)-6-cyclohexyl-4-(methoxymethyl)-4H-thieno[3,2-b]pyrrole-2-carboxylate

HRID 505796
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HRID 505796 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:12][C:11]3[CH:13]=[C:14]([C:16]([O:18][CH3:19])=[O:17])[S:15][C:10]=3[C:9]=2[CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)=[CH:4][CH:3]=1.[H-].[Na+].[CH3:28][O:29][CH2:30]Cl>CN(C=O)C>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[N:12]([CH2:28][O:29][CH3:30])[C:11]3[CH:13]=[C:14]([C:16]([O:18][CH3:19])=[O:17])[S:15][C:10]=3[C:9]=2[CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][CH2:21]2)=[CH:6][CH:7]=1
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참가 물질

5

반응물 3

HCID 7864Chloromethyl Methyl EtherHCID 24758Sodium hydrideHCID 68472408methyl 5-(4-chlorophenyl)-6-cyclohexyl-4H-thieno[3,2-b]pyrrole-2-carboxylate

생성물 1

HCID 68471433methyl 5-(4-chlorophenyl)-6-cyclohexyl-4-(methoxymethyl)-4H-thieno[3,2-b]pyrrole-2-carboxylate수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide
용매

실험 절차

A solution (0.20 M) of methyl 5-(4-chlorophenyl)-6-cyclohexyl-4H-thieno[3,2-b]pyrrole-2-carboxylate in DMF was treated at 0° C. with NaH (1.5 eq., 60% dispersion in mineral oil), and the suspension was stirred at RT for 45 min then cooled again to 0° C., and treated with chloromethyl methyl ether (5 eq.). The reaction mixture was stirred at RT for 1.5 h then was cooled at 0° C. and quenched with aqueous NaHCO3 (saturated solution) and extracted with AcOEt. The combined organic phase was washed with brine and dried. Evaporation of the solvent under reduced pressure gave a residue that was purified by flash chromatography on silica gel (1:9 acetone/toluene) to afford methyl 5-(4-chlorophenyl)-6-cyclohexyl-4-(methoxymethyl)-4H-thieno[3,2-b]pyrrole-2-carboxylate (100%). This compound was dissolved in THF/MeOH (2:3), and the resulting solution (0.08 M) was treated at RT with aqueous NaOH (2N solution, 5 eq.). The mixture was heated at 85° C. for 1.5 h. After cooling down, the reaction mixture was concentrated and acidified to pH 1 with aqueous HCl (1 N) and extracted with AcOEt. The combined organic phase was washed with brine and dried. Evaporation of the solvent under reduced pressure afforded the title compound (96%) as a solid.

후처리

  1. temperaturethen cooled again to 0° C.
  2. stirringThe reaction mixture was stirred at RT for 1.5 h
  3. temperaturethen was cooled at 0° C.
  4. customquenched with aqueous NaHCO3 (saturated solution)
  5. extractionextracted with AcOEt
  6. washThe combined organic phase was washed with brine
  7. customdried
  8. customEvaporation of the solvent under reduced pressure
  9. customgave a residue that
  10. customwas purified by flash chromatography on silica gel (1:9 acetone/toluene)

출처 및 근거

ORD 기록
ord-d66321c879394b34b16b50d7212b748e
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07781431B2

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