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Tri-o-tolylphosphine → HCID 21830726, 화합물

HRID 1600947
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HRID 1600947 반응식
[N:1]1[CH:6]=[CH:5][CH:4]=[C:3]([CH2:7][CH2:8][CH:9]([OH:12])[CH:10]=[CH2:11])[CH:2]=1.[Cl:13][C:14]1[CH:15]=[C:16]([C:20]2[CH:25]=[CH:24][C:23](OS(C(F)(F)F)(=O)=O)=[CH:22][CH:21]=2)[CH:17]=[CH:18][CH:19]=1.C1(C)C=CC=CC=1P(C1C=CC=CC=1C)C1C=CC=CC=1C>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.C(N(CC)CC)C>[Cl:13][C:14]1[CH:15]=[C:16]([C:20]2[CH:21]=[CH:22][C:23]([CH2:11][CH2:10][C:9](=[O:12])[CH2:8][CH2:7][C:3]3[CH:2]=[N:1][CH:6]=[CH:5][CH:4]=3)=[CH:24][CH:25]=2)[CH:17]=[CH:18][CH:19]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

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HCID 80271Tri-o-tolylphosphineHCID 17866850HCID 17866850, 화합물HCID 218306693′-Chloro[1,1′-biphenyl]-4-yl 1,1,1-trifluoromethanesulfonate

생성물 1

HCID 21830726HCID 21830726, 화합물수율 28.7%

시약·촉매·용매 2

HCID 167845palladium(II) acetate촉매
HCID 8471
Triethylamine
용매

실험 절차

Prepared according to the method described in Example 7b) from (±)-5-(3-pyridyl)-1-penten-3-ol (Example 7a, 0.66 g), 3'-chloro-4-trifluoromethanesulfonyloxybiphenyl (1.34 g), palladium(II) acetate (0.09 g), tri-o-tolylphosphine (5 ml) and triethylamine (1 ml) at 80° C. for 5 hours. Work up and purification by column chromatography over silica eluting with dichloromethane:methanol (19:1) gave (±)-1-(3'-chlorobiphenyl-4-yl)-5-(3-pyridyl)-3-pentanone (0.4 g). The latter was immediately dissolved in methanol (10 ml), cooled to 0° C. and sodium borohydride (0.043 g) added. The reaction mixture was stirred at 25° C. for 2 hours and was then concentrated under reduced pressure. Water was added to the residue and the mixture extracted with ethyl acetate. The combined extracts were dried over anhydrous magnesium sulfate, filtered and concentrated under reduced pressure. The residue was purified by column chromatography over silica eluting with ethyl acetate. Conversion to the oxalate salt upon treatment with excess saturated ethereal oxalic acid gave the title compound as a solid (0.094 g).

후처리

  1. customPrepared
  2. customat 80° C.
  3. customfor 5 hours
  4. customWork up and purification by column chromatography over silica eluting with dichloromethane:methanol (19:1)

출처 및 근거

ORD 기록
ord-b97096d5b6124a3d969e8eb2be589e0f
출처 데이터셋
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05977105

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