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Indole-3-Acetic Acid → (1H-Indol-3-yl)-acetic acid 4-dimethylamino-4-phenyl-cyclohexyl ester hydrochloride

HRID 1349398
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HRID 1349398 반응식
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[C:3]([CH2:10][C:11]([OH:13])=[O:12])=[CH:2]1.[CH3:14][N:15]([CH3:29])[C:16]1([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH2:21][CH2:20][CH:19](O)[CH2:18][CH2:17]1.C1(N=C=NC2CCCCC2)CCCCC1.[Cl:45][Si](C)(C)C>CN(C)C1C=CN=CC=1.CC(=O)CC.O.C1COCC1.ClCCl>[ClH:45].[CH3:14][N:15]([CH3:29])[C:16]1([C:23]2[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=2)[CH2:17][CH2:18][CH:19]([O:12][C:11](=[O:13])[CH2:10][C:3]2[C:4]3[C:9](=[CH:8][CH:7]=[CH:6][CH:5]=3)[NH:1][CH:2]=2)[CH2:20][CH2:21]1
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참가 물질

10

반응물 4

HCID 802Indole-3-Acetic AcidHCID 6397ChlorotrimethylsilaneHCID 10868DicyclohexylcarbodiimideHCID 111487094-Dimethylamino-4-phenylcyclohexanol

생성물 1

HCID 69423004(1H-Indol-3-yl)-acetic acid 4-dimethylamino-4-phenyl-cyclohexyl ester hydrochloride

시약·촉매·용매 5

HCID 14284
4-(Dimethylamino)pyridine
촉매
HCID 962Water용매
HCID 6344Dichloromethane용매
HCID 6569Methyl Ethyl Ketone용매
HCID 8028Tetrahydrofuran용매

실험 절차

175 mg of (1H-indol-3-yl)-acetic acid and 219 mg of 4-dimethylamino-4-phenyl-cyclohexanol (mixture of diastereoisomers analogously to Example 4) were added, under argon and while cooling with ice, to a mixture of 5 ml of dry dichloromethane and 5 ml of dry THF with 206 mg of dicyclohexylcarbodiimide and 12 mg of 4-dimethylaminopyridine, and stirring was carried out overnight. The resulting solid was filtered and washed with a small amount of diethyl ether. The resulting filtrate was concentrated and the residue was stirred for five minutes with a mixture of 10 ml of each of two molar sodium hydrogen carbonate solution and ethyl acetate. The phases were separated, the aqueous phase was extracted three times using 10 ml of ethyl acetate each time, and the combined organic phases were washed with 10 ml of water, dried over sodium sulfate and concentrated. The residue obtained was a mixture of the two possible diastereoisomeric esters, which were separated by chromatography on silica gel with methanol. 60 mg of the non-polar and 108 mg of the polar diastereoisomer were obtained in the form of colourless oils which, as described for Example 1, were converted into 65 mg (Example 13) and 118 mg (Example 14) of the corresponding hydrochlorides using chlorotrimethylsilane and water in 2-butanone.

후처리

  1. additionwere added, under argon
  2. filtrationThe resulting solid was filtered
  3. washwashed with a small amount of diethyl ether
  4. concentrationThe resulting filtrate was concentrated
  5. stirringthe residue was stirred for five minutes with a mixture of 10 ml of each of two molar sodium hydrogen carbonate solution and ethyl acetate
  6. customThe phases were separated
  7. extractionthe aqueous phase was extracted three times
  8. washthe combined organic phases were washed with 10 ml of water
  9. dry with materialdried over sodium sulfate
  10. concentrationconcentrated
  11. customThe residue obtained
  12. customwere separated by chromatography on silica gel with methanol
  13. custom60 mg of the non-polar and 108 mg of the polar diastereoisomer were obtained in the form of colourless oils which

출처 및 근거

ORD 기록
ord-3261d23dc5284ec58340677a72786507
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07211694B2

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