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Chloride → HCID 67188901, 화합물

HRID 1254269
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HRID 1254269 반응식
Br[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][Si:9]([C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:11])[CH3:10].[C:16]([Li])(C)(C)C.[CH3:21][O:22]N(C)[C:24]([C@@H:26]1[CH2:31][CH2:30]CN(C(OC(C)(C)C)=O)C1)=[O:25].[Cl-].[NH4+].O(C1C=[CH:54][CH:53]=[CH:52][C:51]=1[C:56]([C@@H:58]1[CH2:63][CH2:62][CH2:61][N:60]([C:64]([O:66][C:67]([CH3:70])([CH3:69])[CH3:68])=[O:65])[CH2:59]1)=[O:57])[Si](C(C)(C)C)(C)C.[OH:71][C:72]1[CH:77]=[CH:76][CH:75]=[CH:74][C:73]=1[C:78]([C@@H:80]1[CH2:85][CH2:84][CH2:83][N:82]([C:86]([O:88][C:89]([CH3:92])([CH3:91])[CH3:90])=[O:87])[CH2:81]1)=[O:79].[Cl-]>CCOCC.O1CCCC1>[OH:57][C@:56]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[O:8][Si:9]([C:12]([CH3:15])([CH3:14])[CH3:13])([CH3:11])[CH3:10])([C@@H:58]1[CH2:63][CH2:62][CH2:61][N:60]([C:64]([O:66][C:67]([CH3:68])([CH3:69])[CH3:70])=[O:65])[CH2:59]1)[CH2:51][CH2:52][CH2:53][CH2:54][O:22][CH3:21].[OH:79][C@:78]([C:73]1[CH:74]=[CH:75][CH:76]=[CH:77][C:72]=1[OH:71])([C@@H:80]1[CH2:85][CH2:84][CH2:83][N:82]([C:86]([O:88][C:89]([CH3:92])([CH3:91])[CH3:90])=[O:87])[CH2:81]1)[CH2:30][CH2:31][CH2:26][CH2:24][O:25][CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

11

반응물 7

HCID 312ChlorideHCID 25517Ammonium ChlorideHCID 11219912(2-Bromophenoxy)(tert-butyl)dimethylsilaneHCID 30025965(R)-tert-butyl 3-(N-methoxy-N-methylcarbamoyl)piperidine-1-carboxylateHCID 67191653HCID 67191653, 화합물HCID 67191868HCID 67191868, 화합물
HCID 178418306
HCID 178418306, 화합물

생성물 2

HCID 67188901HCID 67188901, 화합물수율 47%HCID 67189723HCID 67189723, 화합물수율 45%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매2회HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of bromo-2-[(tert-butyl)dimethylsiloxy]benzene (2.1 g, 7.4 mmol) in Et2O (35 mL) was cooled to −78° C. and treated with 1.7 M tert-butyllithium in hexanes (8.6 mL, 15 mmol). The reaction was stirred for 30 min and a solution of (R)-tert-butyl 3-(N-methoxy-N-methylcarbamoyl)piperidine-1-carboxylate (1.0 g, 3.7 mmol) in Et2O was added slowly. The reaction was allowed to stir and warm to rt over a two hour period. Sat'd aq ammonium chloride was added to quench the reaction. The aq phase was extracted with Et2O three times. The combined organic layers were washed with brine and dried over MgSO4. The solvent was removed by evaporation and the crude product was purified by flash chromatography on silica gel eluting with EtOAc/hexanes to give a mixture of (2-tert-butyldimethylsiloxyphenyl)((R)-N-Boc-piperidin-3-yl)methanone and (2-hydroxyphenyl)((R)-N-Boc-piperidin-3-yl)methanone. A −20° C. solution of the crude mixture in tetrahydrofuran was treated with 1.3 M 4-methoxybutylmagensium chloride in THF (14.9 mL, 19.4 mmol). The reaction was stirred and allowed to warm to rt over a two hour period. The reaction was quenched with ammonium chloride. The aq layer was extracted with Et2O. The combined organic layers were dried over MgSO4 and filtered. The solvent was evaporated and the crude product was purified by flash chromatography on silica gel eluting with EtOAc/hexanes to afford 2-((S)-1-hydroxy-5-methoxy-1-((R)-N-Boc-piperidin-3-yl)pentyl)[tert-butyldimethylsiloxy]benzene (874 mg, 47%) and 2-((S)-1-hydroxy-5-methoxy-1-((R)-N-Boc-piperidin-3-yl)pentyl)phenol (650 mg, 45%).

후처리

  1. stirringto stir
  2. customto quench
  3. customthe reaction
  4. extractionThe aq phase was extracted with Et2O three times
  5. washThe combined organic layers were washed with brine
  6. dry with materialdried over MgSO4
  7. customThe solvent was removed by evaporation
  8. customthe crude product was purified by flash chromatography on silica gel eluting with EtOAc/hexanes
  9. customto give
  10. stirringThe reaction was stirred
  11. temperatureto warm to rt over a two hour period
  12. customThe reaction was quenched with ammonium chloride
  13. extractionThe aq layer was extracted with Et2O
  14. dry with materialThe combined organic layers were dried over MgSO4
  15. filtrationfiltered
  16. customThe solvent was evaporated
  17. customthe crude product was purified by flash chromatography on silica gel eluting with EtOAc/hexanes

출처 및 근거

ORD 기록
ord-7bc8b4a5148b40feb6d8f01c57c4fbf2
출처 데이터셋
uspto-grants-2013_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08455521B2

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