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1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 68679502, 화합물

HRID 2353978
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HRID 2353978 반응식
C(OC(N1C2C(=CC3OC(F)(F)OC=3C=2)[C@H](O)CCC1)=O)(C)(C)C.C1C=CC(P(N=[N+]=[N-])(C2C=CC=CC=2)=O)=CC=1.C1CCN2C(=NCCC2)CC1.[C:53]([O:57][C:58]([N:60]1[C:73]2[C:65](=[CH:66][C:67]3[O:68][C:69]([F:75])([F:74])[O:70][C:71]=3[CH:72]=2)[C@@H:64]([N:76]=[N+]=[N-])[CH2:63][CH2:62][CH2:61]1)=[O:59])([CH3:56])([CH3:55])[CH3:54]>C1(C)C=CC=CC=1.CO.[Pd]>[C:53]([O:57][C:58]([N:60]1[C:73]2[C:65](=[CH:66][C:67]3[O:68][C:69]([F:75])([F:74])[O:70][C:71]=3[CH:72]=2)[C@@H:64]([NH2:76])[CH2:63][CH2:62][CH2:61]1)=[O:59])([CH3:56])([CH3:54])[CH3:55]
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참가 물질

8

반응물 4

HCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 199401P,P-Diphenylphosphinic azideHCID 68679478HCID 68679478, 화합물HCID 86616084(S)-9-Azido-2,2-difluoro-6,7,8,9-tetrahydro-1,3-dioxa-5-aza-cyclohepta[f]indene-5-carboxylic acid tert-butyl ester

생성물 1

HCID 68679502HCID 68679502, 화합물

시약·촉매·용매 3

HCID 23938
Palladium
촉매
HCID 887Methanol용매
HCID 1140Toluene용매

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온도
65 °C

실험 절차

To a solution of (R)-2,2-Difluoro-9-hydroxy-6,7,8,9-tetrahydro-1,3-dioxa-5-aza-cyclohepta[f]indene-5-carboxylic acid tert-butyl ester (1.9 mmol) in Toluene, add DPPA (2.5 mmol) and DBU (2.5 mmol). After heating the mixture at 65° C. for 14 h, remove solvent under vacuum and chromatograph the intermediate using ethyl acetate/hexane (5-20%) to elute. This provides (S)-9-Azido-2,2-difluoro-6,7,8,9-tetrahydro-1,3-dioxa-5-aza-cyclohepta[f]indene-5-carboxylic acid tert-butyl ester as a colorless oil. To a solution of (S)-9-Azido-2,2-difluoro-6,7,8,9-tetrahydro-1,3-dioxa-5-aza-cyclohepta[f]indene-5-carboxylic acid tert-butyl ester (1.8 mmol) in methanol (20 mL) add a catalytic amount of Pd/C after purging the solution with nitrogen. Place a balloon of hydrogen on the reaction and purge the solution several times. After stirring for 1 h, purge the solution with nitrogen then filter through celite. Collect the filtrate and remove solvent under vacuum to provide the title compound as a colorless oil.

후처리

  1. customremove solvent under vacuum and chromatograph the intermediate
  2. washto elute
  3. customafter purging the solution with nitrogen
  4. customon the reaction
  5. custompurge the solution several times
  6. custompurge the solution with nitrogen
  7. filtrationthen filter through celite
  8. customCollect the filtrate
  9. customremove solvent under vacuum

출처 및 근거

ORD 기록
ord-021bfb81ccc3447fb6f8ad890a9eee85
출처 데이터셋
uspto-grants-2010_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07749992B2

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