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Thionyl Chloride → HCID 15660876, 화합물

HRID 344697
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HRID 344697 반응식
ClC(O[CH2:5][CH:6](C)C)=O.[CH3:9][N:10]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[C:11]([CH2:13][CH2:14][C:15]([OH:17])=O)=[O:12].[NH:25]1[CH2:29][CH2:28][CH2:27][C@H:26]1[CH:30]([OH:34])[C:31]([OH:33])=[O:32].S(Cl)(Cl)=O>C1COCC1.C(O)C.C(N(CC)CC)C>[CH2:5]([O:32][C:31](=[O:33])[CH:30]([C@@H:26]1[CH2:27][CH2:28][CH2:29][N:25]1[C:15](=[O:17])[CH2:14][CH2:13][C:11](=[O:12])[N:10]([CH2:18][C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)[CH3:9])[OH:34])[CH3:6]
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참가 물질

8

반응물 4

HCID 24386Thionyl ChlorideHCID 62365Isobutyl chloroformateHCID 845833HCID 845833, 화합물HCID 10844510HCID 10844510, 화합물

생성물 1

HCID 15660876HCID 15660876, 화합물

시약·촉매·용매 3

HCID 702Ethanol용매
HCID 8028
Tetrahydrofuran
용매
HCID 8471Triethylamine용매2회

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온도
-15 °C

실험 절차

Triethylamine (3.5 ml) and isobutyl chloroformate (980 μl) were added to a solution of 3-(N-methyl-N-benzylcarbamoyl) propionic acid (1.33 g) in THF (16 ml). The mixture was stirred for 15 mins at -15° C. The solution was named solution A. (2RS)-2-[(2S)-pyrrolidin-2-yl]-2-hydroxyacetic acid (1.0 g) was dissolved in ethanol (25 ml). The solution was cooled to -20° C. Thionyl chloride (1.0 ml) was added dropwise to the cooled solution. The mixture was stirred for 2 hrs. at room temperature. Triethylamine (5 ml) was added dropwise to the solution cooled to -20° C. again. The solution was allowed to stand to rise to room temperature, and evaporated. THF (26 ml) and triethylamine (1.15 ml) were added to the residue. To the solution cooled to -10° C, the above solution A was added dropwise. The mixture was stirred for 2 hrs at room temperature. Water was added to the reaction solution. The mixture was extracted with EtOAc. The extract was washed, dried and evaporated. The residue was purified by column chromatography on silica gel (hexane-EtOAc) to give the title compound (1.67 g) having the following physical data:

후처리

  1. temperatureThe solution was cooled to -20° C
  2. stirringThe mixture was stirred for 2 hrs
  3. customat room temperature
  4. temperaturecooled to -20° C. again
  5. customto rise to room temperature
  6. customevaporated
  7. additionTHF (26 ml) and triethylamine (1.15 ml) were added to the residue
  8. temperatureTo the solution cooled to -10° C
  9. additionthe above solution A was added dropwise
  10. stirringThe mixture was stirred for 2 hrs at room temperature
  11. additionWater was added to the reaction solution
  12. extractionThe mixture was extracted with EtOAc
  13. washThe extract was washed
  14. customdried
  15. customevaporated
  16. customThe residue was purified by column chromatography on silica gel (hexane-EtOAc)

출처 및 근거

ORD 기록
ord-ccb4157f229245a1989eb6f6a7133c64
출처 데이터셋
uspto-grants-1991_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05053414

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