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Triphenylphosphine → HCID 178454105, 화합물

HRID 707406
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HRID 707406 반응식
[F:1][C:2]1([F:13])[C:10]2[C:5](=[N:6][CH:7]=[C:8]([F:11])[CH:9]=2)[NH:4][C:3]1=[O:12].[C:14]([O:18][C:19](=[O:26])[NH:20][C@H:21]1[CH2:24][C@@H:23](O)[CH2:22]1)([CH3:17])([CH3:16])[CH3:15].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.N(C(OC(C)C)=O)=NC(OC(C)C)=O>C1COCC1.C([O-])(O)=O.[Na+]>[C:14]([O:18][C:19](=[O:26])[NH:20][C@H:21]1[CH2:22][C@H:23]([N:4]2[C:5]3=[N:6][CH:7]=[C:8]([F:11])[CH:9]=[C:10]3[C:2]([F:1])([F:13])[C:3]2=[O:12])[CH2:24]1)([CH3:17])([CH3:15])[CH3:16]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

HCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 847191103,3,5-Trifluoro-1H,2H,3H-pyrrolo[2,3-b]pyridin-2-oneHCID 178454125HCID 178454125, 화합물

생성물 1

HCID 178454105HCID 178454105, 화합물수율 51.2%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
HCID 516892Sodium Bicarbonate용매

실험 절차

3,3,5-Trifluoro-1H-pyrrolo[2,3-b]pyridin-2(3H)-one (0.248 g, 1.318 mmol), tert-butyl(cis-3-hydroxycyclobutyl)carbamate (0.247 g, 1.318 mmol), and triphenylphosphine (0.519 g, 1.978 mmol) were mixed in THF (5 mL) under an argon atmosphere. The mixture was cooled to 0° C. before diisopropyl azodicarboxylate (0.389 mL, 1.978 mmol) was added dropwise via syringe. The reaction mixture was warmed to room temperature and stirred for 22 h. The reaction mixture was diluted with sat. NaHCO3 and extracted with EtOAc. The organic layer was separated, washed with saturated aqueous sodium chloride, dried over magnesium sulfate, filtered, and concentrated in vacuo. The resulting crude product was purified by silica gel column chromatography eluting with EtOAc in hexanes to yield the title compound (0.241 g, 0.674 mmol, 51.2% yield) as a white solid.

후처리

  1. additionwas added dropwise via syringe
  2. extractionextracted with EtOAc
  3. customThe organic layer was separated
  4. washwashed with saturated aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customThe resulting crude product was purified by silica gel column chromatography
  9. washeluting with EtOAc in hexanes

출처 및 근거

ORD 기록
ord-4530ecf4004f4e5abe83dad157ec323f
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09174992B2

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