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Triphenylphosphine → HCID 57748770, 화합물

HRID 1670639
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HRID 1670639 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([NH:8][N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)=[C:4]([N+:16]([O-:18])=[O:17])[CH:3]=1.[F:19][C:20]1[CH:21]=[CH:22][C:23]2=[C:24]([CH:45]=1)[O:25][CH2:26][C:27]1[C:43]([F:44])=[CH:42][CH:41]=[CH:40][C:28]=1/[C:29]/2=[CH:30]\B1OC(C)(C)C(C)(C)O1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.C([O-])(=O)C.[K+]>O1CCOCC1.O.O.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:19][C:20]1[CH:21]=[CH:22][C:23]2=[C:24]([CH:45]=1)[O:25][CH2:26][C:27]1[C:43]([F:44])=[CH:42][CH:41]=[CH:40][C:28]=1/[C:29]/2=[CH:30]\[C:2]1[CH:7]=[CH:6][C:5]([NH:8][N:9]2[CH2:14][CH2:13][N:12]([CH3:15])[CH2:11][CH2:10]2)=[C:4]([N+:16]([O-:18])=[O:17])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 11776TriphenylphosphineHCID 517044Potassium AcetateHCID 67334316HCID 67334316, 화합물HCID 67335785HCID 67335785, 화합물

생성물 1

HCID 57748770HCID 57748770, 화합물수율 55%

시약·촉매·용매 3

HCID 167845
palladium(II) acetate
촉매
HCID 962Water용매
HCID 218864351,4-Dioxane--water (1/1)용매

실험 절차

Degas three times a mixture of (4-bromo-2-nitro-phenyl)-(4-methyl-piperazin-1-yl)-amine (0.016 mol, 5.0 g), (E)-3,7-difluoro-11-(4,4,5,5-tetramethyl[1,3,2]dioxaborolan-2-ylmethylene)-6,11-dihydro-dibenzo[b,e]oxepine (0.017 mol, 6.4 g), triphenylphosphine (0.0028 mol, 0.74 g) and potassium acetate (0.0317 mol, 3.11 g) in dioxane/water (3:1) (200 mL) with nitrogen. Add palladium (II) acetate (0.5 mmol, 113 mg) to the reaction mixture and degas again three times with nitrogen. Heat the resulting reaction mixture at 85° C. for 16 h. Cool the reaction mixture to room temperature and dilute with water. Extract the mixture with ethyl acetate, combine organic layers, and wash with water and brine. Dry the organic phase over anhydrous sodium sulfate, filter, and concentrate. Crystallize the crude material from methanol, filter, and dry under vacuum to obtain the title compound (4.2 g, 55%) as an orange solid. ES-MS m/z 479 [M+1]+.

후처리

  1. customDegas three times
  2. temperatureHeat
  3. customthe resulting reaction mixture at 85° C. for 16 h
  4. extractionExtract the mixture with ethyl acetate
  5. washwash with water and brine
  6. dry with materialDry the organic phase over anhydrous sodium sulfate
  7. filtrationfilter
  8. concentrationconcentrate
  9. customCrystallize the crude material from methanol
  10. filtrationfilter
  11. customdry under vacuum

출처 및 근거

ORD 기록
ord-f4fa6ba0d41f41419c3feeda0dfa86f3
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07994164B2

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