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1,3,5,7-Tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamantane → HCID 178494055, 화합물

HRID 633595
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HRID 633595 반응식
Br[C:2]1[CH:17]=[C:16]([S:18]([N:21]2[CH2:25][CH2:24][CH2:23][CH2:22]2)(=[O:20])=[O:19])[CH:15]=[CH:14][C:3]=1[O:4][C@H:5]1[CH2:10][CH2:9][C@H:8]([N:11]([CH3:13])[CH3:12])[CH2:7][CH2:6]1.C[C:27]12CC3(C)P(C4C=CC=CC=4)[C:33](C)([CH2:35][C:29]([CH3:45])(O3)O1)[O:34]2>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].O1CCOCC1>[CH3:27][O:34][C:33]1[N:11]=[CH:8][CH:7]=[C:29]2[C:45]([C:2]3[CH:17]=[C:16]([S:18]([N:21]4[CH2:25][CH2:24][CH2:23][CH2:22]4)(=[O:20])=[O:19])[CH:15]=[CH:14][C:3]=3[O:4][C@H:5]3[CH2:10][CH2:9][C@H:8]([N:11]([CH3:13])[CH3:12])[CH2:7][CH2:6]3)=[CH:22][N:21]([CH3:25])[C:35]=12
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 534277901,3,5,7-Tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamantaneHCID 178484115HCID 178484115, 화합물

생성물 1

HCID 178494055HCID 178494055, 화합물수율 341.4%

시약·촉매·용매 2

HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 312751,4-Dioxane용매

반응 조건

온도
100 °C

실험 절차

A mixture of Example 144B (60 mg, 0.14 mmol) and Example 59A (40.1 mg, 0.14 mmol) was degassed under argon. To this mixture was added dioxane (8 mL) followed by degassing with argon. To this mixture was added potassium phosphate, dibasic (109 mg, 0.626 mmol) and water (2.000 mL) followed by degassing with argon. To this mixture was added 1,3,5,7-tetramethyl-6-phenyl-2,4,8-trioxa-6-phosphaadamantane (6.91 mg, 0.024 mmol) and then immediately tris(dibenzylideneacetone)dipalladium (0) (8.92 mg, 9.74 μmol) followed by degassing with argon. The reaction mixture was heated at 100° C. for 1 hour. The mixture was cooled to ambient temperature and partitioned between saturated aqueous sodium chloride and ethyl acetate. The organic phase was dried over anhydrous magnesium sulfate, filtered, and concentrated to provide the title compound (0.042 g, 59% yield)

후처리

  1. customby degassing with argon
  2. additionTo this mixture was added potassium phosphate, dibasic (109 mg, 0.626 mmol) and water (2.000 mL)
  3. customby degassing with argon
  4. customby degassing with argon
  5. temperatureThe mixture was cooled to ambient temperature
  6. custompartitioned between saturated aqueous sodium chloride and ethyl acetate
  7. dry with materialThe organic phase was dried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated

출처 및 근거

ORD 기록
ord-d3b156b009b74979a593bb0e8ca551bd
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09321764B2

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